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
Software used to prepare material for publication: PLATON (Spek, 2003).
Crystal data top
Cl0.32O4PPb1.59 | V = 629.68 (1) Å3 |
Mr = 2614.89 | Z = 1 |
Hexagonal, P63/m | F(000) = 1097 |
Hall symbol: -P 6c | Dx = 6.896 Mg m−3 |
a = 9.96350 (2) Å | Synchrotron radiation |
c = 7.32427 (1) Å | T = 296 K |
Data collection top
11BM diffractometer | Detector resolution: 18.4 pixels mm-1 |
Radiation source: synchrotron, synchrotron | |
Refinement top
Least-squares matrix: full | 0 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Pb1 | 0.33333 | 0.66667 | 0.0039 (2) | 0.0104 (1)* | 0.948 (5) |
Pb2 | 0.25449 (7) | 0.00550 (10) | 0.25000 | 0.0104 (1)* | 0.960 (4) |
P | 0.4093 (4) | 0.3773 (4) | 0.25000 | 0.0077 (9)* | |
Cl | 0.00000 | 0.00000 | 0.00000 | 0.0115 (12)* | 0.947 (9) |
O1 | 0.3426 (9) | 0.4905 (8) | 0.25000 | 0.011 (2)* | |
O2 | 0.5897 (9) | 0.4778 (9) | 0.25000 | 0.011 (2)* | |
O3 | 0.3639 (6) | 0.2755 (6) | 0.0784 (6) | 0.0155 (17)* | |
Geometric parameters (Å, º) top
Pb1—O1 | 2.550 (6) | Pb2—O3 | 2.659 (5) |
Pb1—O2i | 2.687 (10) | Pb2—O2ix | 2.326 (11) |
Pb1—O1ii | 2.550 (7) | Pb2—O3x | 2.627 (5) |
Pb1—O2iii | 2.687 (7) | Pb2—O3xi | 2.627 (5) |
Pb1—O1iv | 2.550 (9) | Pb2—O3xii | 2.659 (5) |
Pb1—O2v | 2.687 (8) | P—O1 | 1.570 (10) |
Pb1—O3vi | 2.839 (7) | P—O2 | 1.560 (10) |
Pb1—O3vii | 2.839 (7) | P—O3 | 1.534 (5) |
Pb1—O3viii | 2.839 (6) | P—O3xii | 1.534 (5) |
| | | |
O1—Pb1—O2i | 126.9 (2) | O2v—Pb1—O3viii | 123.3 (2) |
O1—Pb1—O1ii | 75.5 (2) | O3vi—Pb1—O3vii | 115.62 (17) |
O1—Pb1—O2iii | 90.13 (19) | O3vi—Pb1—O3viii | 115.62 (19) |
O1—Pb1—O1iv | 75.5 (3) | O3vii—Pb1—O3viii | 115.6 (2) |
O1—Pb1—O2v | 149.9 (3) | O2ix—Pb2—O3 | 75.1 (3) |
O1—Pb1—O3vi | 83.6 (2) | O3—Pb2—O3x | 136.69 (18) |
O1—Pb1—O3vii | 146.60 (18) | O3—Pb2—O3xi | 82.08 (18) |
O1—Pb1—O3viii | 74.1 (2) | O3—Pb2—O3xii | 56.41 (14) |
O1ii—Pb1—O2i | 149.9 (3) | O2ix—Pb2—O3x | 83.39 (19) |
O2i—Pb1—O2iii | 77.4 (3) | O2ix—Pb2—O3xi | 83.39 (19) |
O1iv—Pb1—O2i | 90.1 (3) | O2ix—Pb2—O3xii | 75.1 (3) |
O2i—Pb1—O2v | 77.4 (3) | O3x—Pb2—O3xi | 132.6 (2) |
O2i—Pb1—O3vi | 123.3 (2) | O3x—Pb2—O3xii | 82.08 (18) |
O2i—Pb1—O3vii | 66.9 (2) | O3xi—Pb2—O3xii | 136.69 (18) |
O2i—Pb1—O3viii | 53.3 (2) | O1—P—O2 | 107.7 (5) |
O1ii—Pb1—O2iii | 126.9 (3) | O1—P—O3 | 112.6 (3) |
O1ii—Pb1—O1iv | 75.5 (3) | O1—P—O3xii | 112.6 (3) |
O1ii—Pb1—O2v | 90.1 (2) | O2—P—O3 | 106.8 (3) |
O1ii—Pb1—O3vi | 74.1 (2) | O2—P—O3xii | 106.8 (3) |
O1ii—Pb1—O3vii | 83.6 (2) | O3—P—O3xii | 110.0 (3) |
O1ii—Pb1—O3viii | 146.6 (2) | Pb1—O1—P | 132.0 (2) |
O1iv—Pb1—O2iii | 149.9 (2) | Pb1—O1—Pb1xiii | 90.0 (3) |
O2iii—Pb1—O2v | 77.4 (2) | Pb1xiii—O1—P | 132.0 (2) |
O2iii—Pb1—O3vi | 53.3 (2) | Pb1xiv—O2—P | 101.7 (3) |
O2iii—Pb1—O3vii | 123.27 (17) | Pb2xv—O2—P | 130.5 (5) |
O2iii—Pb1—O3viii | 66.9 (2) | Pb1vi—O2—P | 101.7 (3) |
O1iv—Pb1—O2v | 126.9 (3) | Pb1xiv—O2—Pb1vi | 87.6 (3) |
O1iv—Pb1—O3vi | 146.6 (2) | Pb2—O3—P | 96.8 (2) |
O1iv—Pb1—O3vii | 74.1 (2) | Pb2—O3—Pb2i | 114.22 (19) |
O1iv—Pb1—O3viii | 83.6 (2) | Pb2i—O3—P | 140.8 (4) |
O2v—Pb1—O3vi | 66.9 (3) | Pb1vi—O3—P | 96.2 (3) |
O2v—Pb1—O3vii | 53.3 (3) | | |
| | | |
O3x—Pb2—O3—P | −17.4 (5) | O3—P—O1—Pb1 | −45.5 (7) |
O3xi—Pb2—O3—P | −165.5 (4) | O1—P—O3—Pb2 | −128.8 (4) |
O3xii—Pb2—O3—P | 1.6 (3) | O2—P—O3—Pb2 | 113.1 (4) |
O3—Pb2—O3xii—P | −1.6 (3) | O3xii—P—O3—Pb2 | −2.4 (5) |
O2—P—O1—Pb1 | 72.0 (5) | O3—P—O3xii—Pb2 | 2.4 (5) |
Symmetry codes: (i) x−y, x, z−1/2; (ii) −y+1, x−y+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+1, −y+1, −z; (vii) y, −x+y+1, −z; (viii) x−y, x, −z; (ix) −y+1, x−y, 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) x−y+1, x, z+1/2; (xv) −x+y+1, −x+1, z. |
Crystal data top
ClO12P3Pb5 | V = 635.02 (1) Å3 |
Mr = 1356.36 | Z = 2 |
Hexagonal, P63/m | F(000) = 1136 |
Hall symbol: -P 6c | Dx = 7.094 Mg m−3 |
a = 9.99497 (2) Å | Synchrotron radiation |
c = 7.33997 (2) Å | T = 296 K |
Data collection top
11BM diffractometer | Detector resolution: 18.4 pixels mm-1 |
Radiation source: synchrotron, synchrotron | |
Refinement top
Least-squares matrix: full | 0 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 | x | y | z | Uiso*/Ueq | |
Pb1 | 0.33333 | 0.66667 | 0.0052 (2) | 0.0241 (2)* | |
Pb2 | 0.25474 (8) | 0.00590 (10) | 0.25000 | 0.0234 (1)* | |
Cl | 0.00000 | 0.00000 | 0.00000 | 0.0141 (12)* | |
P | 0.4098 (5) | 0.3802 (5) | 0.25000 | 0.0150 (12)* | |
O1 | 0.3450 (10) | 0.4920 (10) | 0.25000 | 0.023 (3)* | |
O2 | 0.5890 (10) | 0.4740 (10) | 0.25000 | 0.017 (3)* | |
O3 | 0.3596 (8) | 0.2696 (8) | 0.0814 (8) | 0.030 (2)* | |
Geometric parameters (Å, º) top
Pb1—O1 | 2.548 (7) | Pb2—O3 | 2.610 (7) |
Pb1—O2i | 2.680 (10) | Pb2—Clix | 3.1150 (8) |
Pb1—O1ii | 2.548 (9) | Pb2—O2x | 2.363 (12) |
Pb1—O2iii | 2.680 (7) | Pb2—O3xi | 2.646 (7) |
Pb1—O1iv | 2.548 (11) | Pb2—O3xii | 2.646 (7) |
Pb1—O2v | 2.680 (9) | Pb2—O3xiii | 2.610 (7) |
Pb1—O3vi | 2.877 (9) | P—O1 | 1.547 (11) |
Pb1—O3vii | 2.877 (9) | P—O2 | 1.552 (12) |
Pb1—O3viii | 2.877 (7) | P—O3 | 1.565 (7) |
Pb2—Cl | 3.1150 (8) | P—O3xiii | 1.565 (7) |
| | | |
O1—Pb1—O2i | 127.2 (3) | Clix—Pb2—O2x | 138.34 (14) |
O1—Pb1—O1ii | 75.8 (3) | Clix—Pb2—O3xi | 69.2 (2) |
O1—Pb1—O2iii | 90.5 (2) | Clix—Pb2—O3xii | 136.7 (2) |
O1—Pb1—O1iv | 75.8 (3) | Clix—Pb2—O3xiii | 69.61 (18) |
O1—Pb1—O2v | 150.0 (4) | O2x—Pb2—O3xi | 84.7 (2) |
O1—Pb1—O3vi | 84.2 (3) | O2x—Pb2—O3xii | 84.7 (2) |
O1—Pb1—O3vii | 147.2 (2) | O2x—Pb2—O3xiii | 75.2 (3) |
O1—Pb1—O3viii | 74.3 (2) | O3xi—Pb2—O3xii | 133.7 (3) |
O1ii—Pb1—O2i | 150.0 (4) | O3xi—Pb2—O3xiii | 82.1 (2) |
O2i—Pb1—O2iii | 76.5 (3) | O3xii—Pb2—O3xiii | 137.3 (2) |
O1iv—Pb1—O2i | 90.5 (3) | Pb2—Cl—Pb2i | 91.18 (2) |
O2i—Pb1—O2v | 76.5 (3) | Pb2—Cl—Pb2xiv | 88.82 (2) |
O2i—Pb1—O3vi | 122.3 (3) | Pb2—Cl—Pb2xv | 180.00 |
O2i—Pb1—O3vii | 66.3 (3) | Pb2—Cl—Pb2xvi | 88.82 (2) |
O2i—Pb1—O3viii | 53.5 (2) | Pb2—Cl—Pb2xvii | 91.18 (2) |
O1ii—Pb1—O2iii | 127.2 (3) | Pb2i—Cl—Pb2xiv | 91.18 (2) |
O1ii—Pb1—O1iv | 75.8 (3) | Pb2i—Cl—Pb2xv | 88.82 (2) |
O1ii—Pb1—O2v | 90.5 (3) | Pb2i—Cl—Pb2xvi | 180.00 |
O1ii—Pb1—O3vi | 74.3 (3) | Pb2i—Cl—Pb2xvii | 88.82 (2) |
O1ii—Pb1—O3vii | 84.2 (3) | Pb2xiv—Cl—Pb2xv | 91.18 (2) |
O1ii—Pb1—O3viii | 147.2 (2) | Pb2xiv—Cl—Pb2xvi | 88.82 (2) |
O1iv—Pb1—O2iii | 150.0 (3) | Pb2xiv—Cl—Pb2xvii | 180.00 |
O2iii—Pb1—O2v | 76.5 (3) | Pb2xv—Cl—Pb2xvi | 91.18 (2) |
O2iii—Pb1—O3vi | 53.5 (3) | Pb2xv—Cl—Pb2xvii | 88.82 (2) |
O2iii—Pb1—O3vii | 122.3 (2) | Pb2xvi—Cl—Pb2xvii | 91.18 (2) |
O2iii—Pb1—O3viii | 66.3 (3) | O1—P—O2 | 109.7 (6) |
O1iv—Pb1—O2v | 127.2 (3) | O1—P—O3 | 114.1 (4) |
O1iv—Pb1—O3vi | 147.2 (3) | O1—P—O3xiii | 114.1 (4) |
O1iv—Pb1—O3vii | 74.3 (3) | O2—P—O3 | 107.0 (4) |
O1iv—Pb1—O3viii | 84.2 (3) | O2—P—O3xiii | 107.0 (4) |
O2v—Pb1—O3vi | 66.3 (3) | O3—P—O3xiii | 104.5 (4) |
O2v—Pb1—O3vii | 53.5 (3) | Pb1—O1—P | 132.4 (3) |
O2v—Pb1—O3viii | 122.3 (2) | Pb1—O1—Pb1xviii | 89.7 (3) |
O3vi—Pb1—O3vii | 115.3 (2) | Pb1xviii—O1—P | 132.4 (3) |
O3vi—Pb1—O3viii | 115.3 (3) | Pb1xix—O2—P | 103.5 (3) |
O3vii—Pb1—O3viii | 115.3 (3) | Pb2xx—O2—P | 128.0 (6) |
Cl—Pb2—O3 | 69.61 (18) | Pb1vi—O2—P | 103.5 (3) |
Cl—Pb2—Clix | 72.18 (2) | Pb1xix—O2—Pb2xx | 112.9 (3) |
Cl—Pb2—O2x | 138.34 (14) | Pb1xix—O2—Pb1vi | 88.7 (3) |
Cl—Pb2—O3xi | 136.7 (2) | Pb1vi—O2—Pb2xx | 112.9 (3) |
Cl—Pb2—O3xii | 69.2 (2) | Pb2—O3—P | 99.4 (3) |
Cl—Pb2—O3xiii | 102.13 (18) | Pb2—O3—Pb2i | 115.7 (3) |
Clix—Pb2—O3 | 102.13 (18) | Pb1vi—O3—Pb2 | 100.0 (3) |
O2x—Pb2—O3 | 75.2 (3) | Pb2i—O3—P | 138.1 (4) |
O3—Pb2—O3xi | 137.3 (2) | Pb1vi—O3—P | 95.1 (4) |
O3—Pb2—O3xii | 82.1 (2) | Pb1vi—O3—Pb2i | 100.3 (2) |
O3—Pb2—O3xiii | 56.60 (19) | | |
| | | |
Cl—Pb2—O3—P | 123.2 (5) | O3—P—O1—Pb1 | −47.3 (9) |
O3xi—Pb2—O3—P | −14.8 (7) | O1—P—O3—Pb2 | −128.5 (4) |
O3xii—Pb2—O3—P | −166.1 (5) | O2—P—O3—Pb2 | 109.9 (4) |
O3xiii—Pb2—O3—P | 2.3 (4) | O3xiii—P—O3—Pb2 | −3.3 (6) |
O3—Pb2—O3xiii—P | −2.3 (4) | O3—P—O3xiii—Pb2 | 3.3 (6) |
O2—P—O1—Pb1 | 72.7 (6) | | |
Symmetry codes: (i) x−y, x, z−1/2; (ii) −y+1, x−y+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+1, −y+1, −z; (vii) y, −x+y+1, −z; (viii) x−y, x, −z; (ix) x−y, x, z+1/2; (x) −y+1, x−y, z; (xi) y, −x+y, z+1/2; (xii) y, −x+y, −z; (xiii) x, y, −z+1/2; (xiv) −y, x−y, z; (xv) −x, −y, z−1/2; (xvi) −x+y, −x, z; (xvii) y, −x+y, z−1/2; (xviii) −x+y, −x+1, −z+1/2; (xix) x−y+1, x, z+1/2; (xx) −x+y+1, −x+1, z. |
(2profs_mimetite-chin_publ)
top
Crystal data top
As3ClO12Pb5 | V = 677.93 (1) Å3 |
Mr = 1488.21 | Z = 2 |
Hexagonal, P63/m | F(000) = 1244 |
Hall symbol: -P 6c | Dx = 7.291 Mg m−3 |
a = 10.24823 (2) Å | Synchrotron radiation |
c = 7.45339 (2) Å | T = 296 K |
Data collection top
11BM diffractometer | Detector resolution: 18.4 pixels mm-1 |
Radiation source: synchrotron, synchrotron | |
Refinement top
Least-squares matrix: full | 0 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 | x | y | z | Uiso*/Ueq | |
Pb1 | 0.33333 | 0.66667 | 0.5064 (2) | 0.0139 (1)* | |
Pb2 | 0.00500 (9) | 0.25099 (6) | 0.25000 | 0.0139 (1)* | |
As | 0.38380 (10) | 0.40810 (10) | 0.25000 | 0.0047 (3)* | |
Cl | 0.00000 | 0.00000 | 0.00000 | 0.0141 (10)* | |
O1 | 0.4932 (8) | 0.3226 (8) | 0.25000 | 0.013 (2)* | |
O2 | 0.4853 (8) | 0.5986 (9) | 0.25000 | 0.022 (2)* | |
O3 | 0.2735 (6) | 0.3588 (6) | 0.0666 (7) | 0.042 (2)* | |
Geometric parameters (Å, º) top
Pb1—As | 3.5088 (12) | Pb2—Cl | 3.1558 (5) |
Pb1—O2 | 2.766 (7) | Pb2—O3 | 2.761 (6) |
Pb1—O1i | 2.505 (6) | Pb2—Cli | 3.1558 (5) |
Pb1—Asii | 3.5088 (13) | Pb2—O3i | 2.587 (6) |
Pb1—O2ii | 2.766 (8) | Pb2—O1viii | 3.031 (10) |
Pb1—O1iii | 2.505 (6) | Pb2—O2iv | 2.353 (7) |
Pb1—Asiv | 3.5088 (15) | Pb2—O3vii | 2.761 (6) |
Pb1—O2iv | 2.766 (8) | Pb2—O3ix | 2.587 (6) |
Pb1—O1v | 2.505 (7) | As—O1 | 1.734 (9) |
Pb1—O3vi | 2.948 (9) | As—O2 | 1.692 (8) |
Pb1—O3vii | 2.948 (6) | As—O3 | 1.682 (6) |
Pb2—As | 3.3782 (14) | As—O3vii | 1.682 (6) |
| | | |
As—Pb1—O2 | 28.24 (17) | O2iv—Pb2—O3 | 74.8 (3) |
As—Pb1—O1i | 98.98 (18) | O3—Pb2—O3vii | 59.36 (17) |
As—Pb1—Asii | 93.16 (3) | O3—Pb2—O3ix | 80.9 (2) |
As—Pb1—O2ii | 99.62 (17) | Cli—Pb2—O3i | 70.93 (15) |
As—Pb1—O1iii | 93.36 (16) | Cli—Pb2—O1viii | 102.36 (15) |
As—Pb1—Asiv | 93.16 (4) | Cli—Pb2—O2iv | 137.93 (15) |
As—Pb1—O2iv | 65.5 (2) | Cli—Pb2—O3vii | 68.93 (11) |
As—Pb1—O1v | 165.88 (18) | Cli—Pb2—O3ix | 138.64 (12) |
As—Pb1—O3vi | 121.64 (11) | O1viii—Pb2—O3i | 68.11 (18) |
As—Pb1—O3vii | 28.55 (11) | O2iv—Pb2—O3i | 83.22 (17) |
O1i—Pb1—O2 | 125.5 (3) | O3i—Pb2—O3vii | 80.9 (2) |
Asii—Pb1—O2 | 65.48 (16) | O3i—Pb2—O3ix | 131.6 (3) |
O2—Pb1—O2ii | 77.5 (2) | O1viii—Pb2—O2iv | 97.7 (4) |
O1iii—Pb1—O2 | 92.0 (2) | O1viii—Pb2—O3vii | 148.86 (13) |
Asiv—Pb1—O2 | 99.62 (15) | O1viii—Pb2—O3ix | 68.11 (18) |
O2—Pb1—O2iv | 77.5 (3) | O2iv—Pb2—O3vii | 74.8 (3) |
O1v—Pb1—O2 | 152.4 (3) | O2iv—Pb2—O3ix | 83.22 (17) |
O2—Pb1—O3vi | 125.29 (18) | O3vii—Pb2—O3ix | 138.2 (2) |
O2—Pb1—O3vii | 56.3 (2) | Pb1—As—Pb2 | 77.98 (2) |
Asii—Pb1—O1i | 165.88 (13) | Pb1—As—O1 | 139.31 (14) |
O1i—Pb1—O2ii | 152.4 (3) | Pb1—As—O2 | 50.7 (2) |
O1i—Pb1—O1iii | 73.3 (3) | Pb1—As—O3 | 109.8 (2) |
Asiv—Pb1—O1i | 93.4 (2) | Pb1—As—Pb1vi | 66.00 (3) |
O1i—Pb1—O2iv | 92.0 (2) | Pb1—As—O3vii | 56.88 (19) |
O1i—Pb1—O1v | 73.3 (2) | Pb2—As—O1 | 129.7 (3) |
O1i—Pb1—O3vi | 86.8 (3) | Pb2—As—O2 | 116.6 (3) |
O1i—Pb1—O3vii | 70.5 (2) | Pb2—As—O3 | 54.4 (2) |
Asii—Pb1—O2ii | 28.2 (2) | Pb1vi—As—Pb2 | 77.98 (2) |
Asii—Pb1—O1iii | 98.98 (16) | Pb2—As—O3vii | 54.4 (2) |
Asii—Pb1—Asiv | 93.16 (4) | O1—As—O2 | 113.8 (4) |
Asii—Pb1—O2iv | 99.62 (13) | O1—As—O3 | 110.8 (2) |
Asii—Pb1—O1v | 93.36 (19) | Pb1vi—As—O1 | 139.31 (14) |
Asii—Pb1—O3vi | 93.00 (11) | O1—As—O3vii | 110.8 (2) |
Asii—Pb1—O3vii | 121.64 (12) | O2—As—O3 | 106.2 (3) |
O1iii—Pb1—O2ii | 125.5 (3) | Pb1vi—As—O2 | 50.7 (2) |
Asiv—Pb1—O2ii | 65.5 (2) | O2—As—O3vii | 106.2 (3) |
O2ii—Pb1—O2iv | 77.5 (2) | Pb1vi—As—O3 | 56.88 (19) |
O1v—Pb1—O2ii | 92.0 (2) | O3—As—O3vii | 108.7 (3) |
O2ii—Pb1—O3vi | 66.1 (3) | Pb1vi—As—O3vii | 109.8 (2) |
O2ii—Pb1—O3vii | 125.29 (19) | Pb2—Cl—Pb2x | 91.32 (2) |
Asiv—Pb1—O1iii | 165.88 (16) | Pb2—Cl—Pb2viii | 88.69 (2) |
O1iii—Pb1—O2iv | 152.4 (2) | Pb2—Cl—Pb2xi | 180.00 |
O1iii—Pb1—O1v | 73.3 (3) | Pb2—Cl—Pb2xii | 88.69 (2) |
O1iii—Pb1—O3vi | 142.32 (19) | Pb2—Cl—Pb2xiii | 91.32 (2) |
O1iii—Pb1—O3vii | 86.8 (2) | Pb2x—Cl—Pb2viii | 91.32 (2) |
Asiv—Pb1—O2iv | 28.2 (2) | Pb2x—Cl—Pb2xi | 88.69 (2) |
Asiv—Pb1—O1v | 99.0 (2) | Pb2x—Cl—Pb2xii | 180.00 |
Asiv—Pb1—O3vi | 28.55 (10) | Pb2x—Cl—Pb2xiii | 88.69 (2) |
Asiv—Pb1—O3vii | 93.00 (13) | Pb2viii—Cl—Pb2xi | 91.32 (2) |
O1v—Pb1—O2iv | 125.5 (3) | Pb2viii—Cl—Pb2xii | 88.69 (2) |
O2iv—Pb1—O3vi | 56.3 (3) | Pb2viii—Cl—Pb2xiii | 180.00 |
O2iv—Pb1—O3vii | 66.1 (2) | Pb2xi—Cl—Pb2xii | 91.32 (2) |
O1v—Pb1—O3vi | 70.5 (2) | Pb2xi—Cl—Pb2xiii | 88.69 (2) |
O1v—Pb1—O3vii | 142.3 (2) | Pb2xii—Cl—Pb2xiii | 91.32 (2) |
O3vi—Pb1—O3vii | 116.67 (17) | Pb1xiv—O1—As | 127.0 (2) |
As—Pb2—Cl | 86.27 (2) | Pb2xii—O1—As | 99.6 (3) |
As—Pb2—O3 | 29.69 (12) | Pb1xv—O1—As | 127.0 (2) |
As—Pb2—Cli | 86.27 (2) | Pb1xiv—O1—Pb2xii | 103.3 (2) |
As—Pb2—O3i | 109.55 (17) | Pb1xiv—O1—Pb1xv | 92.9 (3) |
As—Pb2—O1viii | 169.24 (19) | Pb1xv—O1—Pb2xii | 103.3 (2) |
As—Pb2—O2iv | 71.5 (3) | Pb1—O2—As | 101.1 (3) |
As—Pb2—O3vii | 29.69 (12) | Pb1—O2—Pb2ii | 115.5 (2) |
As—Pb2—O3ix | 109.55 (17) | Pb1—O2—Pb1vi | 87.4 (3) |
Cl—Pb2—O3 | 68.93 (11) | Pb2ii—O2—As | 128.1 (5) |
Cl—Pb2—Cli | 72.38 (1) | Pb1vi—O2—As | 101.1 (3) |
Cl—Pb2—O3i | 138.64 (12) | Pb1vi—O2—Pb2ii | 115.5 (2) |
Cl—Pb2—O1viii | 102.36 (15) | Pb2—O3—As | 95.9 (2) |
Cl—Pb2—O2iv | 137.93 (15) | Pb2—O3—Pb2xiii | 115.1 (2) |
Cl—Pb2—O3vii | 103.02 (13) | Pb1vi—O3—Pb2 | 98.7 (2) |
Cl—Pb2—O3ix | 70.93 (15) | Pb2xiii—O3—As | 140.5 (4) |
Cli—Pb2—O3 | 103.02 (13) | Pb1vi—O3—As | 94.6 (2) |
O3—Pb2—O3i | 138.2 (2) | Pb1vi—O3—Pb2xiii | 103.55 (18) |
O1viii—Pb2—O3 | 148.86 (13) | | |
| | | |
O2—Pb1—As—Pb2 | −139.9 (3) | Cl—Pb2—O3—As | −122.3 (2) |
O2—Pb1—As—O1 | 81.2 (4) | O3i—Pb2—O3—As | 18.6 (4) |
O2—Pb1—As—O3 | −95.1 (4) | O3vii—Pb2—O3—As | −1.75 (19) |
O3vi—Pb1—As—O3 | 11.6 (2) | O3ix—Pb2—O3—As | 164.7 (3) |
O3vii—Pb1—As—O3 | 99.9 (3) | O3—Pb2—O3vii—Pb1 | 97.3 (2) |
Cl—Pb2—As—Pb1 | 177.56 (2) | O3—Pb2—O3vii—As | 1.75 (19) |
Cl—Pb2—As—O1 | −36.28 (1) | Pb2—As—O2—Pb1 | 44.75 (18) |
Cl—Pb2—As—O2 | 143.72 (1) | O1—As—O2—Pb1 | −135.25 (18) |
Cl—Pb2—As—O3 | 52.2 (2) | O3—As—O2—Pb1 | 102.6 (3) |
O3—Pb2—As—Pb1 | 125.4 (2) | Pb1—As—O3—Pb2 | −57.97 (18) |
O3—Pb2—As—O1 | −88.5 (2) | O1—As—O3—Pb2 | 124.6 (3) |
O3—Pb2—As—O2 | 91.5 (2) | O2—As—O3—Pb2 | −111.4 (3) |
O3—Pb2—As—O3vii | −177.0 (3) | O3vii—As—O3—Pb2 | 2.6 (3) |
O3i—Pb2—As—O3 | −167.0 (3) | O3—As—O3vii—Pb1 | −101.9 (2) |
O3vii—Pb2—As—O3 | 177.0 (3) | O3—As—O3vii—Pb2 | −2.6 (3) |
O3ix—Pb2—As—O3 | −16.1 (3) | | |
Symmetry codes: (i) x−y, x, z+1/2; (ii) −y+1, x−y+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, x−y, z; (ix) x−y, x, −z; (x) x−y, x, z−1/2; (xi) −x, −y, z−1/2; (xii) −x+y, −x, z; (xiii) y, −x+y, z−1/2; (xiv) x−y+1, x, z−1/2; (xv) −x+1, −y+1, −z+1. |
(2profs_vanadinite_publ)
top
Crystal data top
ClO12Pb5V3 | V = 678.07 (1) Å3 |
Mr = 1416.27 | Z = 2 |
Hexagonal, P63/m | F(000) = 1184 |
Hall symbol: -P 6c | Dx = 6.937 Mg m−3 |
a = 10.32464 (2) Å | Synchrotron radiation |
c = 7.34508 (2) Å | T = 296 K |
Data collection top
11BM diffractometer | Detector resolution: 18.4 pixels mm-1 |
Radiation source: synchrotron, synchrotron | |
Refinement top
Least-squares matrix: full | 0 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 | x | y | z | Uiso*/Ueq | |
Pb1 | 0.33333 | 0.66667 | 0.00710 (10) | 0.0137 (1)* | |
Pb2 | 0.25517 (5) | 0.01245 (7) | 0.25000 | 0.0142 (1)* | |
V | 0.4096 (2) | 0.3838 (2) | 0.25000 | 0.0061 (6)* | |
Cl | 0.00000 | 0.00000 | 0.00000 | 0.0125 (8)* | |
O1 | 0.3321 (9) | 0.4985 (8) | 0.25000 | 0.020 (3)* | |
O2 | 0.5987 (8) | 0.4839 (8) | 0.25000 | 0.008 (2)* | |
O3 | 0.3567 (6) | 0.2690 (6) | 0.0633 (6) | 0.0136 (17)* | |
Geometric parameters (Å, º) top
Pb1—O1 | 2.485 (6) | Pb2—O3 | 2.687 (5) |
Pb1—O2i | 2.751 (9) | Pb2—Clix | 3.1608 (5) |
Pb1—O1ii | 2.485 (7) | Pb2—O2x | 2.351 (10) |
Pb1—O2iii | 2.751 (6) | Pb2—O3xi | 2.556 (5) |
Pb1—O1iv | 2.485 (9) | Pb2—O3xii | 2.556 (5) |
Pb1—O2v | 2.751 (7) | Pb2—O3xiii | 2.687 (5) |
Pb1—O3vi | 2.971 (7) | V—O1 | 1.729 (9) |
Pb1—O3vii | 2.971 (7) | V—O2 | 1.692 (9) |
Pb1—O3viii | 2.971 (6) | V—O3 | 1.714 (5) |
Pb2—Cl | 3.1608 (5) | V—O3xiii | 1.714 (5) |
| | | |
O1—Pb1—O2i | 126.7 (2) | Clix—Pb2—O2x | 139.71 (11) |
O1—Pb1—O1ii | 74.2 (3) | Clix—Pb2—O3xi | 71.01 (16) |
O1—Pb1—O2iii | 90.67 (19) | Clix—Pb2—O3xii | 136.11 (17) |
O1—Pb1—O1iv | 74.2 (3) | Clix—Pb2—O3xiii | 69.51 (14) |
O1—Pb1—O2v | 150.4 (3) | O2x—Pb2—O3xi | 84.18 (19) |
O1—Pb1—O3vi | 84.8 (2) | O2x—Pb2—O3xii | 84.18 (19) |
O1—Pb1—O3vii | 142.77 (19) | O2x—Pb2—O3xiii | 76.3 (3) |
O1—Pb1—O3viii | 70.7 (2) | O3xi—Pb2—O3xii | 128.4 (2) |
O1ii—Pb1—O2i | 150.4 (3) | O3xi—Pb2—O3xiii | 82.31 (18) |
O2i—Pb1—O2iii | 78.1 (2) | O3xii—Pb2—O3xiii | 141.74 (19) |
O1iv—Pb1—O2i | 90.7 (3) | O1—V—O2 | 111.7 (4) |
O2i—Pb1—O2v | 78.1 (2) | O1—V—O3 | 112.2 (3) |
O2i—Pb1—O3vi | 126.3 (2) | O1—V—O3xiii | 112.2 (3) |
O2i—Pb1—O3vii | 66.0 (2) | O2—V—O3 | 107.1 (3) |
O2i—Pb1—O3viii | 57.05 (19) | O2—V—O3xiii | 107.1 (3) |
O1ii—Pb1—O2iii | 126.7 (3) | O3—V—O3xiii | 106.3 (3) |
O1ii—Pb1—O1iv | 74.2 (3) | Pb2—Cl—Pb2i | 90.36 (2) |
O1ii—Pb1—O2v | 90.7 (2) | Pb2—Cl—Pb2xiv | 89.64 (2) |
O1ii—Pb1—O3vi | 70.7 (2) | Pb2—Cl—Pb2xv | 180.00 |
O1ii—Pb1—O3vii | 84.8 (3) | Pb2—Cl—Pb2xvi | 89.64 (2) |
O1ii—Pb1—O3viii | 142.8 (2) | Pb2—Cl—Pb2xvii | 90.36 (2) |
O1iv—Pb1—O2iii | 150.4 (2) | Pb2i—Cl—Pb2xiv | 90.36 (2) |
O2iii—Pb1—O2v | 78.1 (2) | Pb2i—Cl—Pb2xv | 89.64 (2) |
O2iii—Pb1—O3vi | 57.1 (2) | Pb2i—Cl—Pb2xvi | 180.00 |
O2iii—Pb1—O3vii | 126.31 (15) | Pb2i—Cl—Pb2xvii | 89.64 (2) |
O2iii—Pb1—O3viii | 66.0 (2) | Pb2xiv—Cl—Pb2xv | 90.36 (2) |
O1iv—Pb1—O2v | 126.7 (3) | Pb2xiv—Cl—Pb2xvi | 89.64 (2) |
O1iv—Pb1—O3vi | 142.8 (2) | Pb2xiv—Cl—Pb2xvii | 180.00 |
O1iv—Pb1—O3vii | 70.7 (2) | Pb2xv—Cl—Pb2xvi | 90.36 (2) |
O1iv—Pb1—O3viii | 84.8 (2) | Pb2xv—Cl—Pb2xvii | 89.64 (2) |
O2v—Pb1—O3vi | 66.0 (2) | Pb2xvi—Cl—Pb2xvii | 90.36 (2) |
O2v—Pb1—O3vii | 57.1 (2) | Pb1—O1—V | 129.5 (3) |
O2v—Pb1—O3viii | 126.31 (17) | Pb1—O1—Pb1xviii | 91.8 (3) |
O3vi—Pb1—O3vii | 117.04 (17) | Pb1xviii—O1—V | 129.5 (3) |
O3vi—Pb1—O3viii | 117.04 (19) | Pb1xix—O2—V | 101.4 (2) |
O3vii—Pb1—O3viii | 117.0 (2) | Pb2xx—O2—V | 129.0 (5) |
Cl—Pb2—O3 | 69.51 (14) | Pb1vi—O2—V | 101.4 (2) |
Cl—Pb2—Clix | 71.04 (1) | Pb1xix—O2—Pb2xx | 114.8 (2) |
Cl—Pb2—O2x | 139.71 (11) | Pb1xix—O2—Pb1vi | 86.7 (2) |
Cl—Pb2—O3xi | 136.11 (17) | Pb1vi—O2—Pb2xx | 114.8 (2) |
Cl—Pb2—O3xii | 71.01 (16) | Pb2—O3—V | 96.1 (2) |
Cl—Pb2—O3xiii | 104.06 (14) | Pb2—O3—Pb2i | 117.6 (2) |
Clix—Pb2—O3 | 104.06 (14) | Pb1vi—O3—Pb2 | 98.9 (2) |
O2x—Pb2—O3 | 76.3 (3) | Pb2i—O3—V | 137.5 (3) |
O3—Pb2—O3xi | 141.74 (19) | Pb1vi—O3—V | 92.8 (3) |
O3—Pb2—O3xii | 82.31 (18) | Pb1vi—O3—Pb2i | 105.68 (17) |
O3—Pb2—O3xiii | 61.38 (14) | | |
| | | |
Cl—Pb2—O3—V | 122.5 (3) | O3—V—O1—Pb1 | −51.7 (6) |
O3xi—Pb2—O3—V | −17.7 (5) | O1—V—O3—Pb2 | −126.6 (3) |
O3xii—Pb2—O3—V | −164.9 (3) | O2—V—O3—Pb2 | 110.5 (3) |
O3xiii—Pb2—O3—V | 2.6 (2) | O3xiii—V—O3—Pb2 | −3.7 (4) |
O3—Pb2—O3xiii—V | −2.6 (2) | O3—V—O3xiii—Pb2 | 3.7 (4) |
O2—V—O1—Pb1 | 68.5 (4) | | |
Symmetry codes: (i) x−y, x, z−1/2; (ii) −y+1, x−y+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+1, −y+1, −z; (vii) y, −x+y+1, −z; (viii) x−y, x, −z; (ix) x−y, x, z+1/2; (x) −y+1, x−y, z; (xi) y, −x+y, z+1/2; (xii) y, −x+y, −z; (xiii) x, y, −z+1/2; (xiv) −y, x−y, z; (xv) −x, −y, z−1/2; (xvi) −x+y, −x, z; (xvii) y, −x+y, z−1/2; (xviii) −x+y, −x+1, −z+1/2; (xix) x−y+1, x, z+1/2; (xx) −x+y+1, −x+1, z. |