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The title compound is a new mineral consisting of sheets made from edge-sharing Cu(OH)4Cl2 and Mg(OH)6 octahedra. The sheets are only weakly linked by O-H-Cl bridges, giving rise to perfect cleavage along (001) and to strong texture effects in powder diffraction measurements. Owing to low bond-valence sums at the Cl sites of Cu3MgCl2(OH)6 and of several related compounds, bond-valence parameters for the H/Cl pair have been refined to R0 = 1.336 and b = 0.53 Å based on the crystal structures of selected hydroxychlorides.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106053870/so5007sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768106053870/so5007sup2.hkl
Contains datablock I

Computing details top

Data collection: Collect (Bruker AXS BV, 1997-2004); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: Jana2000 (Petricek and Dusek, 2000); program(s) used to refine structure: Jana2000 (Petricek and Dusek, 2000); software used to prepare material for publication: Jana2000 (Petricek and Dusek, 2000).

Figures top
[Figure 1]
[Figure 2]
(I) top
Crystal data top
Cl2Cu3H6MgO6Dx = 3.287 Mg m3
Mr = 387.9Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1Cell parameters from 1752 reflections
Hall symbol: -P 3;-2"θ = 3.5–44.6°
a = 6.2733 (4) ŵ = 8.81 mm1
c = 5.7472 (5) ÅT = 293 K
V = 195.88 (2) Å3Irregular, greenish-blue
Z = 10.17 × 0.15 × 0.08 mm
F(000) = 187
Data collection top
Nonius KappaCCD
diffractometer
628 independent reflections
Radiation source: fine-focus sealed X-ray tube562 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.039
ϕ scans, and ω scans with κ offsetsθmax = 44.6°, θmin = 3.5°
Absorption correction: multi-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
h = 1112
Tmin = 0.271, Tmax = 0.401k = 128
8900 measured reflectionsl = 1111
Refinement top
Refinement on F2Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0036I2)
R[F2 > 2σ(F2)] = 0.020(Δ/σ)max = 0.0001
wR(F2) = 0.085Δρmax = 0.45 e Å3
S = 1.14Δρmin = 0.38 e Å3
628 reflectionsExtinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
20 parametersExtinction coefficient: 0.00055 (15)
All H-atom parameters refined
Crystal data top
Cl2Cu3H6MgO6Z = 1
Mr = 387.9Mo Kα radiation
Trigonal, P3m1µ = 8.81 mm1
a = 6.2733 (4) ÅT = 293 K
c = 5.7472 (5) Å0.17 × 0.15 × 0.08 mm
V = 195.88 (2) Å3
Data collection top
Nonius KappaCCD
diffractometer
628 independent reflections
Absorption correction: multi-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
562 reflections with I > 3σ(I)
Tmin = 0.271, Tmax = 0.401Rint = 0.039
8900 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02020 parameters
wR(F2) = 0.085All H-atom parameters refined
S = 1.14Δρmax = 0.45 e Å3
628 reflectionsΔρmin = 0.38 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg10000.0098 (2)
Cu10.5000.01182 (9)
Cl10.6666670.3333330.36355 (8)0.01681 (11)
O10.64810 (15)0.82405 (8)0.15579 (19)0.0116 (2)
H10.203 (2)0.797 (2)0.283 (5)0.025 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0069 (2)0.0069 (2)0.0156 (4)0.00346 (12)00
Cu10.00846 (11)0.00999 (11)0.01751 (15)0.00499 (6)0.00094 (2)0.00187 (5)
Cl10.01819 (14)0.01819 (14)0.0141 (2)0.00910 (7)00
O10.0114 (3)0.0100 (2)0.0138 (4)0.00572 (13)0.0009 (2)0.00044 (11)
Geometric parameters (Å, º) top
Mg1—O1i2.1111 (9)Cu1—O1xiv1.9771 (6)
Mg1—O1ii2.1111 (9)Cu1—H1vii2.32 (2)
Mg1—O1iii2.1111 (10)Cu1—H1ii2.32 (2)
Mg1—O1iv2.1111 (10)Cu1—H1xv2.32 (3)
Mg1—O1v2.1111 (9)Cu1—H1xii2.32 (3)
Mg1—O1vi2.1111 (9)Cl1—H1xvi2.48 (3)
Mg1—H1vii2.74 (2)Cl1—H1xvii2.48 (3)
Mg1—H1viii2.74 (2)Cl1—H1xviii2.48 (3)
Mg1—H1ix2.74 (2)O1—O1ix2.9619 (12)
Mg1—H1x2.74 (2)O1—O1xix2.6195 (13)
Mg1—H1xi2.74 (2)O1—O1v2.9619 (7)
Mg1—H1xii2.74 (2)O1—O1xx2.6195 (14)
Cu1—Cl12.7650 (3)O1—H12.808 (18)
Cu1—Cl1xiii2.7650 (3)O1—H1ix2.808 (15)
Cu1—O1vii1.9771 (9)O1—H1xxi0.79 (3)
Cu1—O1ii1.9771 (9)H1—H1ix2.45 (3)
Cu1—O1iii1.9771 (6)H1—H1xxi2.45 (3)
O1i—Mg1—O1ii180O1xiv—Cu1—O1ii97.02 (4)
O1i—Mg1—O1iii103.31 (3)O1xiv—Cu1—O1iii180
O1i—Mg1—O1iv76.69 (3)O1xiv—Cu1—H1vii160.9 (6)
O1i—Mg1—O1v103.31 (3)O1xiv—Cu1—H1ii19.1 (6)
O1i—Mg1—O1vi76.69 (3)O1xiv—Cu1—H1xv98.7 (5)
O1i—Mg1—H1vii96.5 (4)O1xiv—Cu1—H1xii81.3 (5)
O1i—Mg1—H1viii83.5 (4)H1vii—Cu1—H1ii180
O1i—Mg1—H1ix96.5 (4)H1vii—Cu1—H1xv63.9 (8)
O1i—Mg1—H1x83.5 (4)H1vii—Cu1—H1xii116.1 (8)
O1i—Mg1—H1xi11.3 (6)H1ii—Cu1—H1vii180
O1i—Mg1—H1xii168.7 (6)H1ii—Cu1—H1xv116.1 (8)
O1ii—Mg1—O1i180H1ii—Cu1—H1xii63.9 (8)
O1ii—Mg1—O1iii76.69 (3)H1xv—Cu1—H1vii63.9 (8)
O1ii—Mg1—O1iv103.31 (3)H1xv—Cu1—H1ii116.1 (8)
O1ii—Mg1—O1v76.69 (3)H1xv—Cu1—H1xii180
O1ii—Mg1—O1vi103.31 (3)H1xii—Cu1—H1vii116.1 (8)
O1ii—Mg1—H1vii83.5 (4)H1xii—Cu1—H1ii63.9 (8)
O1ii—Mg1—H1viii96.5 (4)H1xii—Cu1—H1xv180
O1ii—Mg1—H1ix83.5 (4)Cu1—Cl1—Cu1iii69.113 (10)
O1ii—Mg1—H1x96.5 (4)Cu1—Cl1—Cu1xxii69.112 (10)
O1ii—Mg1—H1xi168.7 (6)Cu1—Cl1—H1xvi115.6 (4)
O1ii—Mg1—H1xii11.3 (6)Cu1—Cl1—H1xvii174.0 (5)
O1iii—Mg1—O1i103.31 (3)Cu1—Cl1—H1xviii115.6 (4)
O1iii—Mg1—O1ii76.69 (3)Cu1iii—Cl1—Cu169.113 (10)
O1iii—Mg1—O1iv180Cu1iii—Cl1—Cu1xxii69.112 (10)
O1iii—Mg1—O1v103.31 (3)Cu1iii—Cl1—H1xvi115.6 (4)
O1iii—Mg1—O1vi76.69 (3)Cu1iii—Cl1—H1xvii115.6 (4)
O1iii—Mg1—H1vii11.3 (6)Cu1iii—Cl1—H1xviii174.0 (5)
O1iii—Mg1—H1viii168.7 (6)Cu1xxii—Cl1—Cu169.112 (10)
O1iii—Mg1—H1ix96.5 (5)Cu1xxii—Cl1—Cu1iii69.112 (10)
O1iii—Mg1—H1x83.5 (5)Cu1xxii—Cl1—H1xvi174.0 (5)
O1iii—Mg1—H1xi96.5 (5)Cu1xxii—Cl1—H1xvii115.6 (6)
O1iii—Mg1—H1xii83.5 (5)Cu1xxii—Cl1—H1xviii115.6 (6)
O1iv—Mg1—O1i76.69 (3)H1xvi—Cl1—H1xvii59.4 (7)
O1iv—Mg1—O1ii103.31 (3)H1xvi—Cl1—H1xviii59.4 (7)
O1iv—Mg1—O1iii180H1xvii—Cl1—H1xvi59.4 (7)
O1iv—Mg1—O1v76.69 (3)H1xvii—Cl1—H1xviii59.4 (6)
O1iv—Mg1—O1vi103.31 (3)H1xviii—Cl1—H1xvi59.4 (7)
O1iv—Mg1—H1vii168.7 (6)H1xviii—Cl1—H1xvii59.4 (6)
O1iv—Mg1—H1viii11.3 (6)Mg1xxiii—O1—Cu1xxiv100.16 (3)
O1iv—Mg1—H1ix83.5 (5)Mg1xxiii—O1—Cu1xxii100.16 (4)
O1iv—Mg1—H1x96.5 (5)Mg1xxiii—O1—O1ix141.65 (4)
O1iv—Mg1—H1xi83.5 (5)Mg1xxiii—O1—O1xix51.65 (2)
O1iv—Mg1—H1xii96.5 (5)Mg1xxiii—O1—O1v141.65 (4)
O1v—Mg1—O1i103.31 (3)Mg1xxiii—O1—O1xx51.65 (3)
O1v—Mg1—O1ii76.69 (3)Mg1xxiii—O1—H1152.9 (4)
O1v—Mg1—O1iii103.31 (3)Mg1xxiii—O1—H1ix152.9 (5)
O1v—Mg1—O1iv76.69 (3)Mg1xxiii—O1—H1xxi137.0 (15)
O1v—Mg1—O1vi180Cu1xxiv—O1—Cu1xxii104.98 (4)
O1v—Mg1—H1vii96.5 (4)Cu1xxiv—O1—O1ix41.49 (3)
O1v—Mg1—H1viii83.5 (4)Cu1xxiv—O1—O1xix48.51 (2)
O1v—Mg1—H1ix11.3 (6)Cu1xxiv—O1—O1v92.53 (4)
O1v—Mg1—H1x168.7 (6)Cu1xxiv—O1—O1xx109.89 (5)
O1v—Mg1—H1xi96.5 (4)Cu1xxiv—O1—H154.6 (5)
O1v—Mg1—H1xii83.5 (4)Cu1xxiv—O1—H1ix96.5 (5)
O1vi—Mg1—O1i76.69 (3)Cu1xxiv—O1—H1xxi105.5 (17)
O1vi—Mg1—O1ii103.31 (3)Cu1xxii—O1—Cu1xxiv104.98 (4)
O1vi—Mg1—O1iii76.69 (3)Cu1xxii—O1—O1ix92.53 (3)
O1vi—Mg1—O1iv103.31 (3)Cu1xxii—O1—O1xix109.89 (5)
O1vi—Mg1—O1v180Cu1xxii—O1—O1v41.49 (2)
O1vi—Mg1—H1vii83.5 (4)Cu1xxii—O1—O1xx48.51 (2)
O1vi—Mg1—H1viii96.5 (4)Cu1xxii—O1—H196.5 (4)
O1vi—Mg1—H1ix168.7 (6)Cu1xxii—O1—H1ix54.6 (6)
O1vi—Mg1—H1x11.3 (6)Cu1xxii—O1—H1xxi105.5 (10)
O1vi—Mg1—H1xi83.5 (4)O1ix—O1—O1xix90
O1vi—Mg1—H1xii96.5 (4)O1ix—O1—O1v60.00 (3)
H1vii—Mg1—H1viii180O1ix—O1—O1xx129.20 (4)
H1vii—Mg1—H1ix88.4 (7)O1ix—O1—H115.4 (6)
H1vii—Mg1—H1x91.6 (7)O1ix—O1—H1ix58.2 (5)
H1vii—Mg1—H1xi88.4 (7)O1ix—O1—H1xxi71.1 (17)
H1vii—Mg1—H1xii91.6 (7)O1xix—O1—O1ix90
H1viii—Mg1—H1vii180O1xix—O1—O1v129.20 (5)
H1viii—Mg1—H1ix91.6 (7)O1xix—O1—O1xx78.40 (4)
H1viii—Mg1—H1x88.4 (7)O1xix—O1—H1102.5 (5)
H1viii—Mg1—H1xi91.6 (7)O1xix—O1—H1ix140.2 (6)
H1viii—Mg1—H1xii88.4 (7)O1xix—O1—H1xxi140.4 (12)
H1ix—Mg1—H1vii88.4 (7)O1v—O1—O1ix60.00 (3)
H1ix—Mg1—H1viii91.6 (7)O1v—O1—O1xix129.20 (5)
H1ix—Mg1—H1x180O1v—O1—O1xx90
H1ix—Mg1—H1xi88.4 (6)O1v—O1—H158.2 (3)
H1ix—Mg1—H1xii91.6 (6)O1v—O1—H1ix15.4 (6)
H1x—Mg1—H1vii91.6 (7)O1v—O1—H1xxi71.1 (11)
H1x—Mg1—H1viii88.4 (7)O1xx—O1—O1ix129.20 (4)
H1x—Mg1—H1ix180O1xx—O1—O1xix78.40 (4)
H1x—Mg1—H1xi91.6 (6)O1xx—O1—O1v90
H1x—Mg1—H1xii88.4 (6)O1xx—O1—H1140.2 (5)
H1xi—Mg1—H1vii88.4 (7)O1xx—O1—H1ix102.5 (5)
H1xi—Mg1—H1viii91.6 (7)O1xx—O1—H1xxi140.4 (14)
H1xi—Mg1—H1ix88.4 (6)H1—O1—H1ix51.8 (6)
H1xi—Mg1—H1x91.6 (6)H1—O1—H1xxi55.7 (18)
H1xi—Mg1—H1xii180H1ix—O1—H151.8 (6)
H1xii—Mg1—H1vii91.6 (7)H1ix—O1—H1xxi55.7 (13)
H1xii—Mg1—H1viii88.4 (7)H1xxi—O1—H155.7 (18)
H1xii—Mg1—H1ix91.6 (6)H1xxi—O1—H1ix55.7 (13)
H1xii—Mg1—H1x88.4 (6)Mg1xxiv—H1—Cu1xxiv76.1 (8)
H1xii—Mg1—H1xi180Mg1xxiv—H1—Cu1xxv76.1 (8)
Cl1—Cu1—Cl1xiii180Mg1xxiv—H1—Cl1xvi161.3 (11)
Cl1—Cu1—O1vii88.54 (2)Mg1xxiv—H1—O1119.8 (10)
Cl1—Cu1—O1ii91.46 (2)Mg1xxiv—H1—O1ix31.7 (11)
Cl1—Cu1—O1iii88.54 (3)Mg1xxiv—H1—O1v119.8 (10)
Cl1—Cu1—O1xiv91.46 (3)Mg1xxiv—H1—H1ix134.2 (12)
Cl1—Cu1—H1vii77.4 (5)Mg1xxiv—H1—H1xxi134.2 (12)
Cl1—Cu1—H1ii102.6 (5)Cu1xxiv—H1—Cu1xxv85.2 (10)
Cl1—Cu1—H1xv77.4 (6)Cu1xxiv—H1—Cl1xvi116.8 (7)
Cl1—Cu1—H1xii102.6 (6)Cu1xxiv—H1—O144.1 (3)
Cl1xiii—Cu1—Cl1180Cu1xxiv—H1—O1ix55.3 (12)
Cl1xiii—Cu1—O1vii91.46 (2)Cu1xxiv—H1—O1v89.8 (8)
Cl1xiii—Cu1—O1ii88.54 (2)Cu1xxiv—H1—H1ix98.5 (10)
Cl1xiii—Cu1—O1iii91.46 (3)Cu1xxiv—H1—H1xxi58.0 (8)
Cl1xiii—Cu1—O1xiv88.54 (3)Cu1xxv—H1—Cu1xxiv85.2 (10)
Cl1xiii—Cu1—H1vii102.6 (5)Cu1xxv—H1—Cl1xvi116.8 (7)
Cl1xiii—Cu1—H1ii77.4 (5)Cu1xxv—H1—O189.8 (8)
Cl1xiii—Cu1—H1xv102.6 (6)Cu1xxv—H1—O1ix55.3 (12)
Cl1xiii—Cu1—H1xii77.4 (6)Cu1xxv—H1—O1v44.1 (3)
O1vii—Cu1—O1ii180Cu1xxv—H1—H1ix58.0 (8)
O1vii—Cu1—O1iii97.02 (4)Cu1xxv—H1—H1xxi98.5 (10)
O1vii—Cu1—O1xiv82.98 (4)Cl1xvi—H1—O175.6 (5)
O1vii—Cu1—H1vii81.3 (5)Cl1xvi—H1—O1ix167 (2)
O1vii—Cu1—H1ii98.7 (5)Cl1xvi—H1—O1v75.6 (5)
O1vii—Cu1—H1xv19.1 (7)Cl1xvi—H1—H1ix60.3 (9)
O1vii—Cu1—H1xii160.9 (7)Cl1xvi—H1—H1xxi60.3 (9)
O1ii—Cu1—O1vii180O1—H1—O1ix93.5 (17)
O1ii—Cu1—O1iii82.98 (4)O1—H1—O1v63.7 (4)
O1ii—Cu1—O1xiv97.02 (4)O1—H1—H1ix64.1 (6)
O1ii—Cu1—H1vii98.7 (5)O1—H1—H1xxi15.4 (7)
O1ii—Cu1—H1ii81.3 (5)O1ix—H1—O193.5 (17)
O1ii—Cu1—H1xv160.9 (7)O1ix—H1—O1v93.5 (17)
O1ii—Cu1—H1xii19.1 (7)O1ix—H1—H1ix109 (2)
O1iii—Cu1—O1vii97.02 (4)O1ix—H1—H1xxi109 (2)
O1iii—Cu1—O1ii82.98 (4)O1v—H1—O163.7 (4)
O1iii—Cu1—O1xiv180O1v—H1—O1ix93.5 (17)
O1iii—Cu1—H1vii19.1 (6)O1v—H1—H1ix15.4 (7)
O1iii—Cu1—H1ii160.9 (6)O1v—H1—H1xxi64.1 (6)
O1iii—Cu1—H1xv81.3 (5)H1ix—H1—H1xxi60.0 (6)
O1iii—Cu1—H1xii98.7 (5)H1xxi—H1—H1ix60.0 (6)
O1xiv—Cu1—O1vii82.98 (4)
Symmetry codes: (i) x1, y1, z; (ii) x+1, y+1, z; (iii) y+1, xy, z; (iv) y1, x+y, z; (v) y+1, x+1, z; (vi) y1, x1, z; (vii) x, y1, z; (viii) x, y+1, z; (ix) y+1, xy+1, z; (x) y1, x+y1, z; (xi) x+y1, x, z; (xii) xy+1, x, z; (xiii) x+1, y, z; (xiv) y, x+y, z; (xv) x+y, x, z; (xvi) x+1, y+1, z+1; (xvii) y, x+y, z+1; (xviii) xy+1, x, z+1; (xix) y, x+y+1, z; (xx) y, x, z; (xxi) x+y, x+1, z; (xxii) x+y+1, x+1, z; (xxiii) x+1, y+1, z; (xxiv) x, y+1, z; (xxv) y, xy, z.

Experimental details

Crystal data
Chemical formulaCl2Cu3H6MgO6
Mr387.9
Crystal system, space groupTrigonal, P3m1
Temperature (K)293
a, c (Å)6.2733 (4), 5.7472 (5)
V3)195.88 (2)
Z1
Radiation typeMo Kα
µ (mm1)8.81
Crystal size (mm)0.17 × 0.15 × 0.08
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionMulti-scan
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
Tmin, Tmax0.271, 0.401
No. of measured, independent and
observed [I > 3σ(I)] reflections
8900, 628, 562
Rint0.039
(sin θ/λ)max1)0.987
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.085, 1.14
No. of reflections628
No. of parameters20
No. of restraints?
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.45, 0.38

Computer programs: Collect (Bruker AXS BV, 1997-2004), HKL SCALEPACK (Otwinowski & Minor 1997), HKL DENZO and SCALEPACK (Otwinowski & Minor 1997), Jana2000 (Petricek and Dusek, 2000).

Selected geometric parameters (Å, º) top
Mg1—O1i2.1111 (9)Cl1—H1iii2.48 (3)
Cu1—Cl12.7650 (3)O1—H12.808 (18)
Cu1—O1ii1.9771 (9)O1—H1iv0.79 (3)
O1i—Mg1—O1v180Cu1vi—Cl1—Cu169.113 (10)
O1i—Mg1—O1vi103.31 (3)Cu1vi—Cl1—H1iii115.6 (4)
O1i—Mg1—O1vii76.69 (3)Cu1vi—Cl1—H1x174.0 (5)
Cl1—Cu1—Cl1viii180H1iii—Cl1—H1xi59.4 (7)
Cl1—Cu1—O1ii88.54 (2)Mg1xii—O1—Cu1xiii100.16 (3)
Cl1—Cu1—O1v91.46 (2)Mg1xii—O1—H1iv137.0 (15)
O1ii—Cu1—O1v180Cu1xiii—O1—Cu1xiv104.98 (4)
O1ii—Cu1—O1vi97.02 (4)Cu1xiii—O1—H1iv105.5 (17)
O1ii—Cu1—O1ix82.98 (4)
Symmetry codes: (i) x1, y1, z; (ii) x, y1, z; (iii) x+1, y+1, z+1; (iv) x+y, x+1, z; (v) x+1, y+1, z; (vi) y+1, xy, z; (vii) y1, x+y, z; (viii) x+1, y, z; (ix) y, x+y, z; (x) xy+1, x, z+1; (xi) y, x+y, z+1; (xii) x+1, y+1, z; (xiii) x, y+1, z; (xiv) x+y+1, x+1, z.
 

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