Crystal structure of polymeric bis­(3-amino-1H-pyrazole)­cadmium dibromide

The title compound {[CdBr₂(3-apz)₂]}_n consists of a Cd²⁺ cation, bromide anions balancing the charge and bridging 3-amino­pyrazole (3-apz) mol­ecules. The Cd²⁺ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN₄Br₂ octa­hedra, and are linked into chains by pairs of the bridging ligands. In the crystal, the 3-apz ligands and bromide anions of neighboring chains are linked through inter­chain hydrogen bonding into a two-dimensional supra­molecular network.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.015 Å
• R factor = 0.045
• wR factor = 0.134
• Data-to-parameter ratio = 15.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............      0.015 Ang.
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      3.313 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         13 Report
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.76Ang From N3      .       0.53 eA-3

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          3 Report
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.20 Why ?
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1       (II)      .       1.92 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        100 Note
PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File          4 Note
PLAT941_ALERT_3_G Average HKL Measurement Multiplicity ...........        4.7 Low
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          0 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  11 ALERT level G = General information/check it is not something unexpected

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   4 ALERT type 5 Informative message, check

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Computing details

catena-Poly[[dibromidocadmium(II)]-bis(µ-3-amino-1H-pyrazole)-κ²N³:N²;κ²N²:N³]

Crystal data

[CdBr2(C3H5N3)2]	Z = 1
Mr = 438.42	F(000) = 206
Triclinic, P1	Dx = 2.492 Mg m^−3
a = 5.0515 (2) Å	Cu Kα radiation, λ = 1.54184 Å
b = 6.7912 (3) Å	Cell parameters from 4554 reflections
c = 8.7083 (6) Å	θ = 5.2–76.6°
α = 83.585 (4)°	µ = 22.83 mm^−1
β = 79.907 (4)°	T = 293 K
γ = 86.833 (3)°	Needle, clear light colourless
V = 292.09 (3) Å^3	0.15 × 0.02 × 0.02 mm

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	1122 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source	1114 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.036
Detector resolution: 10.0000 pixels mm^-1	θmax = 76.8°, θmin = 5.2°
ω scans	h = −6→6
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2020)	k = −8→8
Tmin = 0.212, Tmax = 1.000	l = −10→10
5241 measured reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.045	w = 1/[σ^2(Fo^2) + (0.0297P)^2 + 5.2025P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.134	(Δ/σ)max < 0.001
S = 1.27	Δρmax = 0.94 e Å^−3
1122 reflections	Δρmin = −0.84 e Å^−3
71 parameters	Extinction correction: SHELXL2018/3 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0028 (7)
Primary atom site location: dual

Special details

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.

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

	x	y	z	Uiso*/Ueq
Cd1	1.000000	0.500000	0.500000	0.0316 (4)
Br1	0.9072 (2)	0.25426 (18)	0.28787 (13)	0.0413 (4)
N2	0.3030 (18)	0.6427 (14)	0.1530 (10)	0.037 (2)
H2	0.171982	0.587161	0.125640	0.044*
N1	0.3397 (17)	0.6397 (13)	0.3036 (10)	0.0336 (19)
N3	0.6733 (17)	0.7584 (13)	0.4288 (11)	0.0341 (19)
H3A	0.539337	0.762302	0.509882	0.041*
H3B	0.752934	0.874184	0.416228	0.041*
C3	0.491 (2)	0.7406 (17)	0.0522 (14)	0.040 (2)
H3	0.503093	0.760630	−0.056213	0.048*
C2	0.664 (2)	0.8068 (16)	0.1397 (13)	0.036 (2)
H2A	0.818189	0.878515	0.103040	0.043*
C1	0.559 (2)	0.7436 (15)	0.2937 (12)	0.032 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.0268 (6)	0.0368 (6)	0.0324 (6)	−0.0077 (4)	−0.0069 (4)	−0.0032 (4)
Br1	0.0427 (7)	0.0449 (7)	0.0387 (7)	−0.0148 (5)	−0.0056 (5)	−0.0109 (5)
N2	0.031 (5)	0.048 (5)	0.032 (5)	−0.007 (4)	−0.008 (4)	−0.003 (4)
N1	0.026 (4)	0.040 (5)	0.036 (5)	−0.010 (4)	−0.004 (4)	−0.002 (4)
N3	0.030 (4)	0.033 (4)	0.043 (5)	−0.009 (4)	−0.014 (4)	−0.003 (4)
C3	0.040 (6)	0.042 (6)	0.038 (6)	−0.006 (5)	−0.009 (5)	0.001 (5)
C2	0.032 (5)	0.035 (6)	0.041 (6)	−0.007 (4)	−0.007 (5)	0.003 (4)
C1	0.031 (5)	0.035 (5)	0.032 (5)	0.000 (4)	−0.009 (4)	−0.002 (4)

Geometric parameters (Å, º)

Cd1—Br1^i	2.7379 (11)	N1—C1	1.332 (13)
Cd1—Br1	2.7379 (11)	N3—H3A	0.8900
Cd1—N1^ii	2.358 (9)	N3—H3B	0.8900
Cd1—N1^iii	2.358 (9)	N3—C1	1.413 (13)
Cd1—N3	2.446 (9)	C3—H3	0.9300
Cd1—N3^i	2.446 (9)	C3—C2	1.380 (15)
N2—H2	0.8600	C2—H2A	0.9300
N2—N1	1.355 (12)	C2—C1	1.382 (15)
N2—C3	1.326 (15)
Br1—Cd1—Br1^i	180.0	N2—N1—Cd1^iv	117.1 (6)
N1^iii—Cd1—Br1^i	92.6 (2)	C1—N1—Cd1^iv	138.2 (7)
N1^ii—Cd1—Br1	92.6 (2)	C1—N1—N2	104.1 (8)
N1^ii—Cd1—Br1^i	87.4 (2)	Cd1—N3—H3A	107.7
N1^iii—Cd1—Br1	87.4 (2)	Cd1—N3—H3B	107.7
N1^ii—Cd1—N1^iii	180.0	H3A—N3—H3B	107.1
N1^iii—Cd1—N3^i	88.8 (3)	C1—N3—Cd1	118.3 (7)
N1^ii—Cd1—N3	88.8 (3)	C1—N3—H3A	107.7
N1^ii—Cd1—N3^i	91.2 (3)	C1—N3—H3B	107.7
N1^iii—Cd1—N3	91.2 (3)	N2—C3—H3	126.7
N3—Cd1—Br1^i	85.2 (2)	N2—C3—C2	106.5 (10)
N3^i—Cd1—Br1	85.2 (2)	C2—C3—H3	126.7
N3^i—Cd1—Br1^i	94.8 (2)	C3—C2—H2A	127.4
N3—Cd1—Br1	94.8 (2)	C3—C2—C1	105.1 (10)
N3^i—Cd1—N3	180.0	C1—C2—H2A	127.4
N1—N2—H2	123.6	N1—C1—N3	120.3 (9)
C3—N2—H2	123.6	N1—C1—C2	111.5 (9)
C3—N2—N1	112.7 (9)	C2—C1—N3	127.8 (10)
Cd1^iv—N1—C1—N3	14.7 (16)	N2—C3—C2—C1	−1.1 (13)
Cd1^iv—N1—C1—C2	−172.3 (8)	N1—N2—C3—C2	0.1 (13)
Cd1—N3—C1—N1	87.2 (11)	C3—N2—N1—Cd1^iv	173.9 (7)
Cd1—N3—C1—C2	−84.6 (12)	C3—N2—N1—C1	0.9 (12)
N2—N1—C1—N3	−174.6 (9)	C3—C2—C1—N1	1.7 (13)
N2—N1—C1—C2	−1.6 (12)	C3—C2—C1—N3	174.1 (10)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···Br1^iv	0.86	2.80	3.377 (9)	126
N3—H3A···Br1^ii	0.89	2.61	3.484 (9)	169
N3—H3B···Br1^v	0.89	2.79	3.640 (9)	160

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

Hydrogen-bond geometry (Å, °).

D—H···A	H···A	D···A	D—H···A
N2H···Br^i	3.377 (1)	2.803 (1)	125.63 (1)
N3–H···Br^ii	3.848 (1)	2.607 (1)	168.92 (1)
N3–H···Br^iii	3.640 (1)	2.791 (1)	159.89 (1)

Symmetry codes: (i) 1+x,y,z; (ii) 1-x,1-y,1-z; (iii) x,1+y,z