Inversion parameter of the CoGa2O4 spinel determined from single-crystal X-ray data

Nakatsuka, A.; Ikeda, Y.; Nakayama, N.; Mizota, T.

doi:10.1107/S1600536806011044

Inversion parameter of the CoGa₂O₄ spinel determined from single-crystal X-ray data

A. Nakatsuka, Y. Ikeda, N. Nakayama and T. Mizota

Single crystals of cobalt digallium tetraoxide, CoGa₂O₄, have been grown by cooling slowly a 1:1 mixture of CoO and Ga₂O₃ from 1473 K to room temperature under the presence of a PbF₂ flux. The compound crystallizes with the cubic spinel structure (space group Fd $\overline{3}$ m). The occupancy refinement based on single-crystal X-ray diffraction data shows CoGa₂O₄ to be a largely normal spinel with an inversion parameter of 0.575 (4), resulting in a structural formula of ^IV(Co_0.425Ga_0.575)^VI[Co_0.575Ga_1.425]O₄, where ^IV() and ^VI[] represent the tetrahedral and the octahedral sites, respectively.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806011044/wm2007sup1.cif Contains datablocks General, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806011044/wm2007Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 296 K
Mean () = 0.000 Å
Disorder in main residue
R factor = 0.017
wR factor = 0.023
Data-to-parameter ratio = 23.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT301_ALERT_3_B Main Residue  Disorder .........................      39.00 Perc.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.25 Ratio
PLAT128_ALERT_4_C Non-standard setting of Space group         ....    Fd-3m
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT711_ALERT_1_C BOND    Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    O      CO1/GA1O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    O      CO2/GA2O
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O      CO/GA2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O      CO/GA2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO1/GA1
                    CO1/GA1O      CO/GA2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O      CO/GA2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O      CO/GA2
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........    CO2/GA2
                    CO2/GA2O      CO/GA2

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           60.00
           From the CIF: _reflns_number_total                248
           Count of symmetry unique reflns            0
           Completeness (_total/calc)      Infinity    %
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       248
           Fraction of Friedel pairs measured Infinity
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   8 ALERT level B = Potentially serious problem
  40 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

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

Computing details top

Data collection: WinAFC (Rigaku Corporation, 1999); cell refinement: WinAFC; data reduction: RADY (Sasaki, 1987); program(s) used to solve structure: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to refine structure: RADY; molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: TEXSAN.

cobalt digallium tetraoxide top

Crystal data top

CoGa₂O₄	D_x = 6.034 Mg m⁻³
M_r = 262.37	Mo Kα radiation, λ = 0.71069 Å
Cubic, Fd3m	Cell parameters from 38 reflections
Hall symbol: -F 4vw 2vw 3	θ = 20.0–24.7°
a = 8.3281 (3) Å	µ = 24.01 mm⁻¹
V = 577.61 (4) Å³	T = 296 K
Z = 8	Prism, dark blue
F(000) = 968	0.13 × 0.11 × 0.09 mm

Data collection top

Rigaku AFC-7R diffractometer	R_int = 0.023
ω–2θ scans	θ_max = 60.0°
Absorption correction: ψ scan (North et al., 1968)	h = 0→20
T_min = 0.060, T_max = 0.115	k = 0→20
613 measured reflections	l = 0→20
248 independent reflections	3 standard reflections every 100 reflections
215 reflections with F > 3σ(F)	intensity decay: 1.0%

Refinement top

Refinement on F	w = 1/σ²(F)
R[F² > 2σ(F²)] = 0.017	(Δ/σ)_max = 0.00008
wR(F²) = 0.023	Δρ_max = 0.84 e Å⁻³
S = 1.72	Δρ_min = −0.43 e Å⁻³
215 reflections	Extinction correction: isotropic Type I (Becker & Coppens, 1974a,b)
9 parameters	Extinction coefficient: 3.06 (6)×10^-4

Special details top

Refinement. Refinement using reflections with F > 3.0 σ(F). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F > 3.0 σ(F) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.1250	0.1250	0.1250	0.00373 (1)	0.425
Ga1	0.1250	0.1250	0.1250	0.00373	0.575 (4)
Co2	0.5000	0.5000	0.5000	0.00353 (1)	0.288
Ga2	0.5000	0.5000	0.5000	0.00353	0.712
O	0.25842 (19)	0.25842	0.25842	0.00760 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.00373 (12)	0.00373	0.00373	0.00000	0.00000	0.00000
Ga1	0.00373	0.00373	0.00373	0.00000	0.00000	0.00000
Co2	0.00353 (9)	0.00353	0.00353	−0.00040 (7)	−0.00040	−0.00040
Ga2	0.00353	0.00353	0.00353	−0.00040	−0.00040	−0.00040
O	0.0076 (3)	0.0076	0.0076	0.0002 (4)	0.0002	0.0002

Geometric parameters (Å, º) top

Co1/Ga1—O	1.9245 (16)	Co2/Ga2—O^ix	2.0144 (16)
Co1/Ga1—Oⁱ	1.9245 (16)	O—Oⁱⁱ	3.143 (3)
Co1/Ga1—Oⁱⁱ	1.9245 (16)	O—Oⁱⁱⁱ	3.143 (3)
Co1/Ga1—Oⁱⁱⁱ	1.9245 (16)	O—O^ix	2.746 (3)
Co2/Ga2—O^iv	2.0144 (16)	O—O^viii	2.746 (3)
Co2/Ga2—O^v	2.0144 (16)	O—O^x	2.9478 (16)
Co2/Ga2—O^vi	2.0144 (16)	O—O^xi	2.9478 (16)
Co2/Ga2—O^vii	2.0144 (16)	O—O^xii	2.9478 (16)
Co2/Ga2—O^viii	2.0144 (16)	O—O^xiii	2.9478 (16)

O—Co1/Ga1—Oⁱ	109.47 (10)	O^viii—Co2/Ga2—O^iv	94.06 (9)
O—Co1/Ga1—Oⁱⁱ	109.47 (10)	O^vii—Co2/Ga2—O^vi	94.06 (7)
O—Co1/Ga1—Oⁱⁱⁱ	109.47 (10)	O^vii—Co2/Ga2—O^v	94.06 (9)
Oⁱⁱ—Co1/Ga1—Oⁱ	109.47 (10)	O^vii—Co2/Ga2—O^iv	180.00
Oⁱⁱⁱ—Co1/Ga1—Oⁱ	109.47 (10)	O^vi—Co2/Ga2—O^v	85.94 (7)
Oⁱⁱⁱ—Co1/Ga1—Oⁱⁱ	109.47 (10)	O^vi—Co2/Ga2—O^iv	85.94 (7)
O^ix—Co2/Ga2—O^viii	85.94 (7)	O^v—Co2/Ga2—O^iv	85.94 (7)
O^ix—Co2/Ga2—O^vii	85.94 (7)	Co1/Ga1—O—Co/Ga2^xiv	122.44 (8)
O^ix—Co2/Ga2—O^vi	179.97	Co1/Ga1—O—Co/Ga2^xv	122.44 (8)
O^ix—Co2/Ga2—O^v	94.06 (7)	Co1/Ga1—O—Co/Ga2^xvi	122.44 (8)
O^ix—Co2/Ga2—O^iv	94.06 (7)	Co2/Ga2^xiv—O—Co/Ga2^xv	93.92 (7)
O^viii—Co2/Ga2—O^vii	85.94 (7)	Co2/Ga2^xiv—O—Co/Ga2^xvi	93.92 (7)
O^viii—Co2/Ga2—O^vi	94.06 (7)	Co2/Ga2^xv—O—Co/Ga2^xvi	93.92 (7)
O^viii—Co2/Ga2—O^v	179.97

Symmetry codes: (i) x, −y+1/4, −z+1/4; (ii) −x+1/4, y, −z+1/4; (iii) −x+1/4, −y+1/4, z; (iv) −x+1, y+1/4, z+1/4; (v) x+1/4, −y+1, z+1/4; (vi) x+1/4, y+1/4, −z+1; (vii) x, −y+3/4, −z+3/4; (viii) −x+3/4, y, −z+3/4; (ix) −x+3/4, −y+3/4, z; (x) x−1/4, y+1/4, −z+1/2; (xi) x+1/4, y−1/4, −z+1/2; (xii) x+1/4, −y+1/2, z−1/4; (xiii) x−1/4, −y+1/2, z+1/4; (xiv) x−1/4, y−1/4, −z+1; (xv) x−1/4, −y+1, z−1/4; (xvi) −x+1, y−1/4, z−1/4.

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