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The crystal structure of four Pb apatite samples, Pb5(BO4)3Cl, was refined with synchrotron high-resolution powder X-ray diffraction data, Rietveld refinements, space group P63/m and Z = 2. For this isotypic series, B = P5+ is pyromorphite, B = As5+ is mimetite and B = V5+ is vanadinite. The ionic radius for As5+ (0.355 Å) is similar to that of V5+ (0.335 Å), and this is twice as large as that for P5+ (0.170 Å). However, the c unit-cell parameter for mimetite is surprisingly different from that of vanadinite, although their unit-cell volumes, V, are almost equal to each other. No explanation was available for this peculiar c-axis value for mimetite. Structural parameters such as average 〈B—O〉 [4], 〈Pb1—O9〉 [9] and 〈Pb2—O6Cl2〉 [8] distances increase linearly with V (the coordination numbers for the cations are given in square brackets). Mimetite has a short Pb2—O1 distance, so the O1 oxygen atom interacts with the 6s2 lone-pair electrons of the Pb2+ cation that causes the Cl—Cl distance (= c/2) to increase to the largest value in the series because of repulsion, which causes the c-axis to increase anomalously. Although Pb apatite minerals occur naturally in ore deposits, they are also formed as scaly deposits in lead water pipes that give rise to lead in tap water, as was found recently in Flint, Michigan, USA. It is important to identify Pb-containing phases in water-pipe deposits.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600577517014217/co5089sup1.cif
Contains datablocks global, pyromor_ch_publ

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600577517014217/co5089sup2.cif
Contains datablocks global, pyromorphite_publ

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600577517014217/co5089sup3.cif
Contains datablocks global, 2profs_mimetite-chin_publ

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600577517014217/co5089sup4.cif
Contains datablocks global, 2profs_vanadinite_publ

Computing details top

Software used to prepare material for publication: PLATON (Spek, 2003).

(pyromor_ch_publ) top
Crystal data top
Cl0.32O4PPb1.59V = 629.68 (1) Å3
Mr = 2614.89Z = 1
Hexagonal, P63/mF(000) = 1097
Hall symbol: -P 6cDx = 6.896 Mg m3
a = 9.96350 (2) ÅSynchrotron radiation
c = 7.32427 (1) ÅT = 296 K
Data collection top
11BM
diffractometer
Detector resolution: 18.4 pixels mm-1
Radiation source: synchrotron, synchrotron
Refinement top
Least-squares matrix: full0 restraints
49498 data points(Δ/σ)max = 0.030
36 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pb10.333330.666670.0039 (2)0.0104 (1)*0.948 (5)
Pb20.25449 (7)0.00550 (10)0.250000.0104 (1)*0.960 (4)
P0.4093 (4)0.3773 (4)0.250000.0077 (9)*
Cl0.000000.000000.000000.0115 (12)*0.947 (9)
O10.3426 (9)0.4905 (8)0.250000.011 (2)*
O20.5897 (9)0.4778 (9)0.250000.011 (2)*
O30.3639 (6)0.2755 (6)0.0784 (6)0.0155 (17)*
Geometric parameters (Å, º) top
Pb1—O12.550 (6)Pb2—O32.659 (5)
Pb1—O2i2.687 (10)Pb2—O2ix2.326 (11)
Pb1—O1ii2.550 (7)Pb2—O3x2.627 (5)
Pb1—O2iii2.687 (7)Pb2—O3xi2.627 (5)
Pb1—O1iv2.550 (9)Pb2—O3xii2.659 (5)
Pb1—O2v2.687 (8)P—O11.570 (10)
Pb1—O3vi2.839 (7)P—O21.560 (10)
Pb1—O3vii2.839 (7)P—O31.534 (5)
Pb1—O3viii2.839 (6)P—O3xii1.534 (5)
O1—Pb1—O2i126.9 (2)O2v—Pb1—O3viii123.3 (2)
O1—Pb1—O1ii75.5 (2)O3vi—Pb1—O3vii115.62 (17)
O1—Pb1—O2iii90.13 (19)O3vi—Pb1—O3viii115.62 (19)
O1—Pb1—O1iv75.5 (3)O3vii—Pb1—O3viii115.6 (2)
O1—Pb1—O2v149.9 (3)O2ix—Pb2—O375.1 (3)
O1—Pb1—O3vi83.6 (2)O3—Pb2—O3x136.69 (18)
O1—Pb1—O3vii146.60 (18)O3—Pb2—O3xi82.08 (18)
O1—Pb1—O3viii74.1 (2)O3—Pb2—O3xii56.41 (14)
O1ii—Pb1—O2i149.9 (3)O2ix—Pb2—O3x83.39 (19)
O2i—Pb1—O2iii77.4 (3)O2ix—Pb2—O3xi83.39 (19)
O1iv—Pb1—O2i90.1 (3)O2ix—Pb2—O3xii75.1 (3)
O2i—Pb1—O2v77.4 (3)O3x—Pb2—O3xi132.6 (2)
O2i—Pb1—O3vi123.3 (2)O3x—Pb2—O3xii82.08 (18)
O2i—Pb1—O3vii66.9 (2)O3xi—Pb2—O3xii136.69 (18)
O2i—Pb1—O3viii53.3 (2)O1—P—O2107.7 (5)
O1ii—Pb1—O2iii126.9 (3)O1—P—O3112.6 (3)
O1ii—Pb1—O1iv75.5 (3)O1—P—O3xii112.6 (3)
O1ii—Pb1—O2v90.1 (2)O2—P—O3106.8 (3)
O1ii—Pb1—O3vi74.1 (2)O2—P—O3xii106.8 (3)
O1ii—Pb1—O3vii83.6 (2)O3—P—O3xii110.0 (3)
O1ii—Pb1—O3viii146.6 (2)Pb1—O1—P132.0 (2)
O1iv—Pb1—O2iii149.9 (2)Pb1—O1—Pb1xiii90.0 (3)
O2iii—Pb1—O2v77.4 (2)Pb1xiii—O1—P132.0 (2)
O2iii—Pb1—O3vi53.3 (2)Pb1xiv—O2—P101.7 (3)
O2iii—Pb1—O3vii123.27 (17)Pb2xv—O2—P130.5 (5)
O2iii—Pb1—O3viii66.9 (2)Pb1vi—O2—P101.7 (3)
O1iv—Pb1—O2v126.9 (3)Pb1xiv—O2—Pb1vi87.6 (3)
O1iv—Pb1—O3vi146.6 (2)Pb2—O3—P96.8 (2)
O1iv—Pb1—O3vii74.1 (2)Pb2—O3—Pb2i114.22 (19)
O1iv—Pb1—O3viii83.6 (2)Pb2i—O3—P140.8 (4)
O2v—Pb1—O3vi66.9 (3)Pb1vi—O3—P96.2 (3)
O2v—Pb1—O3vii53.3 (3)
O3x—Pb2—O3—P17.4 (5)O3—P—O1—Pb145.5 (7)
O3xi—Pb2—O3—P165.5 (4)O1—P—O3—Pb2128.8 (4)
O3xii—Pb2—O3—P1.6 (3)O2—P—O3—Pb2113.1 (4)
O3—Pb2—O3xii—P1.6 (3)O3xii—P—O3—Pb22.4 (5)
O2—P—O1—Pb172.0 (5)O3—P—O3xii—Pb22.4 (5)
Symmetry codes: (i) xy, x, z1/2; (ii) y+1, xy+1, z; (iii) x+1, y+1, z1/2; (iv) x+y, x+1, z; (v) y, x+y+1, z1/2; (vi) x+1, y+1, z; (vii) y, x+y+1, z; (viii) xy, x, z; (ix) y+1, xy, z; (x) y, x+y, z+1/2; (xi) y, x+y, z; (xii) x, y, z+1/2; (xiii) x+y, x+1, z+1/2; (xiv) xy+1, x, z+1/2; (xv) x+y+1, x+1, z.
 
(pyromorphite_publ) top
Crystal data top
ClO12P3Pb5V = 635.02 (1) Å3
Mr = 1356.36Z = 2
Hexagonal, P63/mF(000) = 1136
Hall symbol: -P 6cDx = 7.094 Mg m3
a = 9.99497 (2) ÅSynchrotron radiation
c = 7.33997 (2) ÅT = 296 K
Data collection top
11BM
diffractometer
Detector resolution: 18.4 pixels mm-1
Radiation source: synchrotron, synchrotron
Refinement top
Least-squares matrix: full0 restraints
49497 data points(Δ/σ)max = 0.010
33 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.333330.666670.0052 (2)0.0241 (2)*
Pb20.25474 (8)0.00590 (10)0.250000.0234 (1)*
Cl0.000000.000000.000000.0141 (12)*
P0.4098 (5)0.3802 (5)0.250000.0150 (12)*
O10.3450 (10)0.4920 (10)0.250000.023 (3)*
O20.5890 (10)0.4740 (10)0.250000.017 (3)*
O30.3596 (8)0.2696 (8)0.0814 (8)0.030 (2)*
Geometric parameters (Å, º) top
Pb1—O12.548 (7)Pb2—O32.610 (7)
Pb1—O2i2.680 (10)Pb2—Clix3.1150 (8)
Pb1—O1ii2.548 (9)Pb2—O2x2.363 (12)
Pb1—O2iii2.680 (7)Pb2—O3xi2.646 (7)
Pb1—O1iv2.548 (11)Pb2—O3xii2.646 (7)
Pb1—O2v2.680 (9)Pb2—O3xiii2.610 (7)
Pb1—O3vi2.877 (9)P—O11.547 (11)
Pb1—O3vii2.877 (9)P—O21.552 (12)
Pb1—O3viii2.877 (7)P—O31.565 (7)
Pb2—Cl3.1150 (8)P—O3xiii1.565 (7)
O1—Pb1—O2i127.2 (3)Clix—Pb2—O2x138.34 (14)
O1—Pb1—O1ii75.8 (3)Clix—Pb2—O3xi69.2 (2)
O1—Pb1—O2iii90.5 (2)Clix—Pb2—O3xii136.7 (2)
O1—Pb1—O1iv75.8 (3)Clix—Pb2—O3xiii69.61 (18)
O1—Pb1—O2v150.0 (4)O2x—Pb2—O3xi84.7 (2)
O1—Pb1—O3vi84.2 (3)O2x—Pb2—O3xii84.7 (2)
O1—Pb1—O3vii147.2 (2)O2x—Pb2—O3xiii75.2 (3)
O1—Pb1—O3viii74.3 (2)O3xi—Pb2—O3xii133.7 (3)
O1ii—Pb1—O2i150.0 (4)O3xi—Pb2—O3xiii82.1 (2)
O2i—Pb1—O2iii76.5 (3)O3xii—Pb2—O3xiii137.3 (2)
O1iv—Pb1—O2i90.5 (3)Pb2—Cl—Pb2i91.18 (2)
O2i—Pb1—O2v76.5 (3)Pb2—Cl—Pb2xiv88.82 (2)
O2i—Pb1—O3vi122.3 (3)Pb2—Cl—Pb2xv180.00
O2i—Pb1—O3vii66.3 (3)Pb2—Cl—Pb2xvi88.82 (2)
O2i—Pb1—O3viii53.5 (2)Pb2—Cl—Pb2xvii91.18 (2)
O1ii—Pb1—O2iii127.2 (3)Pb2i—Cl—Pb2xiv91.18 (2)
O1ii—Pb1—O1iv75.8 (3)Pb2i—Cl—Pb2xv88.82 (2)
O1ii—Pb1—O2v90.5 (3)Pb2i—Cl—Pb2xvi180.00
O1ii—Pb1—O3vi74.3 (3)Pb2i—Cl—Pb2xvii88.82 (2)
O1ii—Pb1—O3vii84.2 (3)Pb2xiv—Cl—Pb2xv91.18 (2)
O1ii—Pb1—O3viii147.2 (2)Pb2xiv—Cl—Pb2xvi88.82 (2)
O1iv—Pb1—O2iii150.0 (3)Pb2xiv—Cl—Pb2xvii180.00
O2iii—Pb1—O2v76.5 (3)Pb2xv—Cl—Pb2xvi91.18 (2)
O2iii—Pb1—O3vi53.5 (3)Pb2xv—Cl—Pb2xvii88.82 (2)
O2iii—Pb1—O3vii122.3 (2)Pb2xvi—Cl—Pb2xvii91.18 (2)
O2iii—Pb1—O3viii66.3 (3)O1—P—O2109.7 (6)
O1iv—Pb1—O2v127.2 (3)O1—P—O3114.1 (4)
O1iv—Pb1—O3vi147.2 (3)O1—P—O3xiii114.1 (4)
O1iv—Pb1—O3vii74.3 (3)O2—P—O3107.0 (4)
O1iv—Pb1—O3viii84.2 (3)O2—P—O3xiii107.0 (4)
O2v—Pb1—O3vi66.3 (3)O3—P—O3xiii104.5 (4)
O2v—Pb1—O3vii53.5 (3)Pb1—O1—P132.4 (3)
O2v—Pb1—O3viii122.3 (2)Pb1—O1—Pb1xviii89.7 (3)
O3vi—Pb1—O3vii115.3 (2)Pb1xviii—O1—P132.4 (3)
O3vi—Pb1—O3viii115.3 (3)Pb1xix—O2—P103.5 (3)
O3vii—Pb1—O3viii115.3 (3)Pb2xx—O2—P128.0 (6)
Cl—Pb2—O369.61 (18)Pb1vi—O2—P103.5 (3)
Cl—Pb2—Clix72.18 (2)Pb1xix—O2—Pb2xx112.9 (3)
Cl—Pb2—O2x138.34 (14)Pb1xix—O2—Pb1vi88.7 (3)
Cl—Pb2—O3xi136.7 (2)Pb1vi—O2—Pb2xx112.9 (3)
Cl—Pb2—O3xii69.2 (2)Pb2—O3—P99.4 (3)
Cl—Pb2—O3xiii102.13 (18)Pb2—O3—Pb2i115.7 (3)
Clix—Pb2—O3102.13 (18)Pb1vi—O3—Pb2100.0 (3)
O2x—Pb2—O375.2 (3)Pb2i—O3—P138.1 (4)
O3—Pb2—O3xi137.3 (2)Pb1vi—O3—P95.1 (4)
O3—Pb2—O3xii82.1 (2)Pb1vi—O3—Pb2i100.3 (2)
O3—Pb2—O3xiii56.60 (19)
Cl—Pb2—O3—P123.2 (5)O3—P—O1—Pb147.3 (9)
O3xi—Pb2—O3—P14.8 (7)O1—P—O3—Pb2128.5 (4)
O3xii—Pb2—O3—P166.1 (5)O2—P—O3—Pb2109.9 (4)
O3xiii—Pb2—O3—P2.3 (4)O3xiii—P—O3—Pb23.3 (6)
O3—Pb2—O3xiii—P2.3 (4)O3—P—O3xiii—Pb23.3 (6)
O2—P—O1—Pb172.7 (6)
Symmetry codes: (i) xy, x, z1/2; (ii) y+1, xy+1, z; (iii) x+1, y+1, z1/2; (iv) x+y, x+1, z; (v) y, x+y+1, z1/2; (vi) x+1, y+1, z; (vii) y, x+y+1, z; (viii) xy, x, z; (ix) xy, x, z+1/2; (x) y+1, xy, z; (xi) y, x+y, z+1/2; (xii) y, x+y, z; (xiii) x, y, z+1/2; (xiv) y, xy, z; (xv) x, y, z1/2; (xvi) x+y, x, z; (xvii) y, x+y, z1/2; (xviii) x+y, x+1, z+1/2; (xix) xy+1, x, z+1/2; (xx) x+y+1, x+1, z.
 
(2profs_mimetite-chin_publ) top
Crystal data top
As3ClO12Pb5V = 677.93 (1) Å3
Mr = 1488.21Z = 2
Hexagonal, P63/mF(000) = 1244
Hall symbol: -P 6cDx = 7.291 Mg m3
a = 10.24823 (2) ÅSynchrotron radiation
c = 7.45339 (2) ÅT = 296 K
Data collection top
11BM
diffractometer
Detector resolution: 18.4 pixels mm-1
Radiation source: synchrotron, synchrotron
Refinement top
Least-squares matrix: full0 restraints
49497 data points(Δ/σ)max = 0.220
35 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.333330.666670.5064 (2)0.0139 (1)*
Pb20.00500 (9)0.25099 (6)0.250000.0139 (1)*
As0.38380 (10)0.40810 (10)0.250000.0047 (3)*
Cl0.000000.000000.000000.0141 (10)*
O10.4932 (8)0.3226 (8)0.250000.013 (2)*
O20.4853 (8)0.5986 (9)0.250000.022 (2)*
O30.2735 (6)0.3588 (6)0.0666 (7)0.042 (2)*
Geometric parameters (Å, º) top
Pb1—As3.5088 (12)Pb2—Cl3.1558 (5)
Pb1—O22.766 (7)Pb2—O32.761 (6)
Pb1—O1i2.505 (6)Pb2—Cli3.1558 (5)
Pb1—Asii3.5088 (13)Pb2—O3i2.587 (6)
Pb1—O2ii2.766 (8)Pb2—O1viii3.031 (10)
Pb1—O1iii2.505 (6)Pb2—O2iv2.353 (7)
Pb1—Asiv3.5088 (15)Pb2—O3vii2.761 (6)
Pb1—O2iv2.766 (8)Pb2—O3ix2.587 (6)
Pb1—O1v2.505 (7)As—O11.734 (9)
Pb1—O3vi2.948 (9)As—O21.692 (8)
Pb1—O3vii2.948 (6)As—O31.682 (6)
Pb2—As3.3782 (14)As—O3vii1.682 (6)
As—Pb1—O228.24 (17)O2iv—Pb2—O374.8 (3)
As—Pb1—O1i98.98 (18)O3—Pb2—O3vii59.36 (17)
As—Pb1—Asii93.16 (3)O3—Pb2—O3ix80.9 (2)
As—Pb1—O2ii99.62 (17)Cli—Pb2—O3i70.93 (15)
As—Pb1—O1iii93.36 (16)Cli—Pb2—O1viii102.36 (15)
As—Pb1—Asiv93.16 (4)Cli—Pb2—O2iv137.93 (15)
As—Pb1—O2iv65.5 (2)Cli—Pb2—O3vii68.93 (11)
As—Pb1—O1v165.88 (18)Cli—Pb2—O3ix138.64 (12)
As—Pb1—O3vi121.64 (11)O1viii—Pb2—O3i68.11 (18)
As—Pb1—O3vii28.55 (11)O2iv—Pb2—O3i83.22 (17)
O1i—Pb1—O2125.5 (3)O3i—Pb2—O3vii80.9 (2)
Asii—Pb1—O265.48 (16)O3i—Pb2—O3ix131.6 (3)
O2—Pb1—O2ii77.5 (2)O1viii—Pb2—O2iv97.7 (4)
O1iii—Pb1—O292.0 (2)O1viii—Pb2—O3vii148.86 (13)
Asiv—Pb1—O299.62 (15)O1viii—Pb2—O3ix68.11 (18)
O2—Pb1—O2iv77.5 (3)O2iv—Pb2—O3vii74.8 (3)
O1v—Pb1—O2152.4 (3)O2iv—Pb2—O3ix83.22 (17)
O2—Pb1—O3vi125.29 (18)O3vii—Pb2—O3ix138.2 (2)
O2—Pb1—O3vii56.3 (2)Pb1—As—Pb277.98 (2)
Asii—Pb1—O1i165.88 (13)Pb1—As—O1139.31 (14)
O1i—Pb1—O2ii152.4 (3)Pb1—As—O250.7 (2)
O1i—Pb1—O1iii73.3 (3)Pb1—As—O3109.8 (2)
Asiv—Pb1—O1i93.4 (2)Pb1—As—Pb1vi66.00 (3)
O1i—Pb1—O2iv92.0 (2)Pb1—As—O3vii56.88 (19)
O1i—Pb1—O1v73.3 (2)Pb2—As—O1129.7 (3)
O1i—Pb1—O3vi86.8 (3)Pb2—As—O2116.6 (3)
O1i—Pb1—O3vii70.5 (2)Pb2—As—O354.4 (2)
Asii—Pb1—O2ii28.2 (2)Pb1vi—As—Pb277.98 (2)
Asii—Pb1—O1iii98.98 (16)Pb2—As—O3vii54.4 (2)
Asii—Pb1—Asiv93.16 (4)O1—As—O2113.8 (4)
Asii—Pb1—O2iv99.62 (13)O1—As—O3110.8 (2)
Asii—Pb1—O1v93.36 (19)Pb1vi—As—O1139.31 (14)
Asii—Pb1—O3vi93.00 (11)O1—As—O3vii110.8 (2)
Asii—Pb1—O3vii121.64 (12)O2—As—O3106.2 (3)
O1iii—Pb1—O2ii125.5 (3)Pb1vi—As—O250.7 (2)
Asiv—Pb1—O2ii65.5 (2)O2—As—O3vii106.2 (3)
O2ii—Pb1—O2iv77.5 (2)Pb1vi—As—O356.88 (19)
O1v—Pb1—O2ii92.0 (2)O3—As—O3vii108.7 (3)
O2ii—Pb1—O3vi66.1 (3)Pb1vi—As—O3vii109.8 (2)
O2ii—Pb1—O3vii125.29 (19)Pb2—Cl—Pb2x91.32 (2)
Asiv—Pb1—O1iii165.88 (16)Pb2—Cl—Pb2viii88.69 (2)
O1iii—Pb1—O2iv152.4 (2)Pb2—Cl—Pb2xi180.00
O1iii—Pb1—O1v73.3 (3)Pb2—Cl—Pb2xii88.69 (2)
O1iii—Pb1—O3vi142.32 (19)Pb2—Cl—Pb2xiii91.32 (2)
O1iii—Pb1—O3vii86.8 (2)Pb2x—Cl—Pb2viii91.32 (2)
Asiv—Pb1—O2iv28.2 (2)Pb2x—Cl—Pb2xi88.69 (2)
Asiv—Pb1—O1v99.0 (2)Pb2x—Cl—Pb2xii180.00
Asiv—Pb1—O3vi28.55 (10)Pb2x—Cl—Pb2xiii88.69 (2)
Asiv—Pb1—O3vii93.00 (13)Pb2viii—Cl—Pb2xi91.32 (2)
O1v—Pb1—O2iv125.5 (3)Pb2viii—Cl—Pb2xii88.69 (2)
O2iv—Pb1—O3vi56.3 (3)Pb2viii—Cl—Pb2xiii180.00
O2iv—Pb1—O3vii66.1 (2)Pb2xi—Cl—Pb2xii91.32 (2)
O1v—Pb1—O3vi70.5 (2)Pb2xi—Cl—Pb2xiii88.69 (2)
O1v—Pb1—O3vii142.3 (2)Pb2xii—Cl—Pb2xiii91.32 (2)
O3vi—Pb1—O3vii116.67 (17)Pb1xiv—O1—As127.0 (2)
As—Pb2—Cl86.27 (2)Pb2xii—O1—As99.6 (3)
As—Pb2—O329.69 (12)Pb1xv—O1—As127.0 (2)
As—Pb2—Cli86.27 (2)Pb1xiv—O1—Pb2xii103.3 (2)
As—Pb2—O3i109.55 (17)Pb1xiv—O1—Pb1xv92.9 (3)
As—Pb2—O1viii169.24 (19)Pb1xv—O1—Pb2xii103.3 (2)
As—Pb2—O2iv71.5 (3)Pb1—O2—As101.1 (3)
As—Pb2—O3vii29.69 (12)Pb1—O2—Pb2ii115.5 (2)
As—Pb2—O3ix109.55 (17)Pb1—O2—Pb1vi87.4 (3)
Cl—Pb2—O368.93 (11)Pb2ii—O2—As128.1 (5)
Cl—Pb2—Cli72.38 (1)Pb1vi—O2—As101.1 (3)
Cl—Pb2—O3i138.64 (12)Pb1vi—O2—Pb2ii115.5 (2)
Cl—Pb2—O1viii102.36 (15)Pb2—O3—As95.9 (2)
Cl—Pb2—O2iv137.93 (15)Pb2—O3—Pb2xiii115.1 (2)
Cl—Pb2—O3vii103.02 (13)Pb1vi—O3—Pb298.7 (2)
Cl—Pb2—O3ix70.93 (15)Pb2xiii—O3—As140.5 (4)
Cli—Pb2—O3103.02 (13)Pb1vi—O3—As94.6 (2)
O3—Pb2—O3i138.2 (2)Pb1vi—O3—Pb2xiii103.55 (18)
O1viii—Pb2—O3148.86 (13)
O2—Pb1—As—Pb2139.9 (3)Cl—Pb2—O3—As122.3 (2)
O2—Pb1—As—O181.2 (4)O3i—Pb2—O3—As18.6 (4)
O2—Pb1—As—O395.1 (4)O3vii—Pb2—O3—As1.75 (19)
O3vi—Pb1—As—O311.6 (2)O3ix—Pb2—O3—As164.7 (3)
O3vii—Pb1—As—O399.9 (3)O3—Pb2—O3vii—Pb197.3 (2)
Cl—Pb2—As—Pb1177.56 (2)O3—Pb2—O3vii—As1.75 (19)
Cl—Pb2—As—O136.28 (1)Pb2—As—O2—Pb144.75 (18)
Cl—Pb2—As—O2143.72 (1)O1—As—O2—Pb1135.25 (18)
Cl—Pb2—As—O352.2 (2)O3—As—O2—Pb1102.6 (3)
O3—Pb2—As—Pb1125.4 (2)Pb1—As—O3—Pb257.97 (18)
O3—Pb2—As—O188.5 (2)O1—As—O3—Pb2124.6 (3)
O3—Pb2—As—O291.5 (2)O2—As—O3—Pb2111.4 (3)
O3—Pb2—As—O3vii177.0 (3)O3vii—As—O3—Pb22.6 (3)
O3i—Pb2—As—O3167.0 (3)O3—As—O3vii—Pb1101.9 (2)
O3vii—Pb2—As—O3177.0 (3)O3—As—O3vii—Pb22.6 (3)
O3ix—Pb2—As—O316.1 (3)
Symmetry codes: (i) xy, x, z+1/2; (ii) y+1, xy+1, z; (iii) x+1, y+1, z+1/2; (iv) x+y, x+1, z; (v) y, x+y+1, z+1/2; (vi) x+y, x+1, z+1/2; (vii) x, y, z+1/2; (viii) y, xy, z; (ix) xy, x, z; (x) xy, x, z1/2; (xi) x, y, z1/2; (xii) x+y, x, z; (xiii) y, x+y, z1/2; (xiv) xy+1, x, z1/2; (xv) x+1, y+1, z+1.
 
(2profs_vanadinite_publ) top
Crystal data top
ClO12Pb5V3V = 678.07 (1) Å3
Mr = 1416.27Z = 2
Hexagonal, P63/mF(000) = 1184
Hall symbol: -P 6cDx = 6.937 Mg m3
a = 10.32464 (2) ÅSynchrotron radiation
c = 7.34508 (2) ÅT = 296 K
Data collection top
11BM
diffractometer
Detector resolution: 18.4 pixels mm-1
Radiation source: synchrotron, synchrotron
Refinement top
Least-squares matrix: full0 restraints
49495 data points(Δ/σ)max = 0.130
35 parameters
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.333330.666670.00710 (10)0.0137 (1)*
Pb20.25517 (5)0.01245 (7)0.250000.0142 (1)*
V0.4096 (2)0.3838 (2)0.250000.0061 (6)*
Cl0.000000.000000.000000.0125 (8)*
O10.3321 (9)0.4985 (8)0.250000.020 (3)*
O20.5987 (8)0.4839 (8)0.250000.008 (2)*
O30.3567 (6)0.2690 (6)0.0633 (6)0.0136 (17)*
Geometric parameters (Å, º) top
Pb1—O12.485 (6)Pb2—O32.687 (5)
Pb1—O2i2.751 (9)Pb2—Clix3.1608 (5)
Pb1—O1ii2.485 (7)Pb2—O2x2.351 (10)
Pb1—O2iii2.751 (6)Pb2—O3xi2.556 (5)
Pb1—O1iv2.485 (9)Pb2—O3xii2.556 (5)
Pb1—O2v2.751 (7)Pb2—O3xiii2.687 (5)
Pb1—O3vi2.971 (7)V—O11.729 (9)
Pb1—O3vii2.971 (7)V—O21.692 (9)
Pb1—O3viii2.971 (6)V—O31.714 (5)
Pb2—Cl3.1608 (5)V—O3xiii1.714 (5)
O1—Pb1—O2i126.7 (2)Clix—Pb2—O2x139.71 (11)
O1—Pb1—O1ii74.2 (3)Clix—Pb2—O3xi71.01 (16)
O1—Pb1—O2iii90.67 (19)Clix—Pb2—O3xii136.11 (17)
O1—Pb1—O1iv74.2 (3)Clix—Pb2—O3xiii69.51 (14)
O1—Pb1—O2v150.4 (3)O2x—Pb2—O3xi84.18 (19)
O1—Pb1—O3vi84.8 (2)O2x—Pb2—O3xii84.18 (19)
O1—Pb1—O3vii142.77 (19)O2x—Pb2—O3xiii76.3 (3)
O1—Pb1—O3viii70.7 (2)O3xi—Pb2—O3xii128.4 (2)
O1ii—Pb1—O2i150.4 (3)O3xi—Pb2—O3xiii82.31 (18)
O2i—Pb1—O2iii78.1 (2)O3xii—Pb2—O3xiii141.74 (19)
O1iv—Pb1—O2i90.7 (3)O1—V—O2111.7 (4)
O2i—Pb1—O2v78.1 (2)O1—V—O3112.2 (3)
O2i—Pb1—O3vi126.3 (2)O1—V—O3xiii112.2 (3)
O2i—Pb1—O3vii66.0 (2)O2—V—O3107.1 (3)
O2i—Pb1—O3viii57.05 (19)O2—V—O3xiii107.1 (3)
O1ii—Pb1—O2iii126.7 (3)O3—V—O3xiii106.3 (3)
O1ii—Pb1—O1iv74.2 (3)Pb2—Cl—Pb2i90.36 (2)
O1ii—Pb1—O2v90.7 (2)Pb2—Cl—Pb2xiv89.64 (2)
O1ii—Pb1—O3vi70.7 (2)Pb2—Cl—Pb2xv180.00
O1ii—Pb1—O3vii84.8 (3)Pb2—Cl—Pb2xvi89.64 (2)
O1ii—Pb1—O3viii142.8 (2)Pb2—Cl—Pb2xvii90.36 (2)
O1iv—Pb1—O2iii150.4 (2)Pb2i—Cl—Pb2xiv90.36 (2)
O2iii—Pb1—O2v78.1 (2)Pb2i—Cl—Pb2xv89.64 (2)
O2iii—Pb1—O3vi57.1 (2)Pb2i—Cl—Pb2xvi180.00
O2iii—Pb1—O3vii126.31 (15)Pb2i—Cl—Pb2xvii89.64 (2)
O2iii—Pb1—O3viii66.0 (2)Pb2xiv—Cl—Pb2xv90.36 (2)
O1iv—Pb1—O2v126.7 (3)Pb2xiv—Cl—Pb2xvi89.64 (2)
O1iv—Pb1—O3vi142.8 (2)Pb2xiv—Cl—Pb2xvii180.00
O1iv—Pb1—O3vii70.7 (2)Pb2xv—Cl—Pb2xvi90.36 (2)
O1iv—Pb1—O3viii84.8 (2)Pb2xv—Cl—Pb2xvii89.64 (2)
O2v—Pb1—O3vi66.0 (2)Pb2xvi—Cl—Pb2xvii90.36 (2)
O2v—Pb1—O3vii57.1 (2)Pb1—O1—V129.5 (3)
O2v—Pb1—O3viii126.31 (17)Pb1—O1—Pb1xviii91.8 (3)
O3vi—Pb1—O3vii117.04 (17)Pb1xviii—O1—V129.5 (3)
O3vi—Pb1—O3viii117.04 (19)Pb1xix—O2—V101.4 (2)
O3vii—Pb1—O3viii117.0 (2)Pb2xx—O2—V129.0 (5)
Cl—Pb2—O369.51 (14)Pb1vi—O2—V101.4 (2)
Cl—Pb2—Clix71.04 (1)Pb1xix—O2—Pb2xx114.8 (2)
Cl—Pb2—O2x139.71 (11)Pb1xix—O2—Pb1vi86.7 (2)
Cl—Pb2—O3xi136.11 (17)Pb1vi—O2—Pb2xx114.8 (2)
Cl—Pb2—O3xii71.01 (16)Pb2—O3—V96.1 (2)
Cl—Pb2—O3xiii104.06 (14)Pb2—O3—Pb2i117.6 (2)
Clix—Pb2—O3104.06 (14)Pb1vi—O3—Pb298.9 (2)
O2x—Pb2—O376.3 (3)Pb2i—O3—V137.5 (3)
O3—Pb2—O3xi141.74 (19)Pb1vi—O3—V92.8 (3)
O3—Pb2—O3xii82.31 (18)Pb1vi—O3—Pb2i105.68 (17)
O3—Pb2—O3xiii61.38 (14)
Cl—Pb2—O3—V122.5 (3)O3—V—O1—Pb151.7 (6)
O3xi—Pb2—O3—V17.7 (5)O1—V—O3—Pb2126.6 (3)
O3xii—Pb2—O3—V164.9 (3)O2—V—O3—Pb2110.5 (3)
O3xiii—Pb2—O3—V2.6 (2)O3xiii—V—O3—Pb23.7 (4)
O3—Pb2—O3xiii—V2.6 (2)O3—V—O3xiii—Pb23.7 (4)
O2—V—O1—Pb168.5 (4)
Symmetry codes: (i) xy, x, z1/2; (ii) y+1, xy+1, z; (iii) x+1, y+1, z1/2; (iv) x+y, x+1, z; (v) y, x+y+1, z1/2; (vi) x+1, y+1, z; (vii) y, x+y+1, z; (viii) xy, x, z; (ix) xy, x, z+1/2; (x) y+1, xy, z; (xi) y, x+y, z+1/2; (xii) y, x+y, z; (xiii) x, y, z+1/2; (xiv) y, xy, z; (xv) x, y, z1/2; (xvi) x+y, x, z; (xvii) y, x+y, z1/2; (xviii) x+y, x+1, z+1/2; (xix) xy+1, x, z+1/2; (xx) x+y+1, x+1, z.
 

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