The structures of polycrystalline Ca3RE2(BO3)4 (RE = La, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Y; space group Pnma) orthoborates were determined using powder X-ray diffraction. Trends in the unit-cell dimensions and yet unreported trends in other structural properties (interatomic distances and the fractional occupation of three Ca/RE sites) for these compounds are demonstrated as a function of RE ionic radius. The unit-cell volume and a unit-cell parameter present a linear dependence, while the b and c unit-cell parameters change in a nonlinear manner. For the whole series, the RE atoms are present at all three cationic sites (labelled as M1, M2 and M3), but the fractional occupancies depend on the RE ionic radius. The small rare-earth atoms tend to enter mainly the M3 site; for the larger rare earths, the occupancy of this site decreases sharply. The occupancy of the M1 site by RE atoms is around 0.5 and tends to increase with increasing RE ionic radius. The M2 site is the least preferentially occupied by RE ions, but the occupancy discernibly increases with rising radius as well. These findings are assembled with properties of isostructural strontium and barium borates, allowing prediction of occupancy schemes for not yet investigated compounds from the A3RE2(BO3)4 (A = Ca, Ba, Sr).
Supporting information
CCDC references: 2036062; 2036063; 2036064; 2036065; 2036066; 2036067; 2036068; 2036069; 2036070; 2036071
Crystal data top
B4Ca3O12La2 | b = 16.0345 (3) Å |
Mr = 633.28 | c = 8.67587 (17) Å |
Orthorhombic, Pnma | V = 1012.35 (3) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.27716 (15) Å | T = 297 K |
Data collection top
PANalytical X'Pert Pro MPD diffractometer | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 4.21 | Rexp = 1.64 |
Rwp = 5.84 | RBragg = 11.7 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.5297 (2) | 0.08586 (10) | 0.8207 (2) | 1.28 (4) | 0.405 (2) |
RE1 | 0.5297 (2) | 0.08586 (10) | 0.8207 (2) | 1.28 (4) | 0.595 (2) |
Ca2 | 0.6883 (3) | 0.12829 (13) | 0.3504 (3) | 1.28 (4) | 0.639 (2) |
RE2 | 0.6883 (3) | 0.12829 (13) | 0.3504 (3) | 1.28 (4) | 0.361 (2) |
Ca3 | 0.3255 (6) | 0.25000 | 0.5256 (5) | 1.28 (4) | 0.911 (4) |
RE3 | 0.3255 (6) | 0.25000 | 0.5256 (5) | 1.28 (4) | 0.089 (4) |
B1 | 0.317 (3) | 0.4540 (11) | 0.4382 (11) | 4.500 | |
B2 | 0.685 (3) | 0.25000 | 0.6553 (14) | 4.500 | |
B3 | 0.487 (4) | 0.25000 | 0.129 (3) | 4.500 | |
O1 | 0.5434 (15) | 0.1736 (5) | 0.0754 (11) | 1.51 (11) | |
O2 | 0.7582 (14) | 0.3216 (5) | 0.7128 (12) | 1.51 (11) | |
O3 | 0.3855 (14) | 0.4069 (6) | 0.5571 (10) | 1.51 (11) | |
O4 | 0.2000 (13) | 0.5157 (6) | 0.4763 (12) | 1.51 (11) | |
O5 | 0.4011 (13) | 0.4492 (6) | 0.2992 (10) | 1.51 (11) | |
O6 | 0.3831 (16) | 0.25000 | 0.2596 (11) | 1.51 (11) | |
O7 | 0.6466 (19) | 0.25000 | 0.5018 (10) | 1.51 (11) | |
Geometric parameters (Å, º) top
RE1—O1i | 2.622 (9) | RE3—O3 | 2.568 (10) |
RE1—O2ii | 2.488 (10) | RE3—O6 | 2.346 (11) |
RE1—O3iii | 2.800 (10) | RE3—O7 | 2.346 (14) |
RE1—O4iii | 2.700 (10) | RE3—O1ix | 2.546 (11) |
RE1—O5iv | 2.477 (10) | RE3—O2ii | 2.590 (11) |
RE1—O4v | 2.425 (10) | RE3—O1x | 2.546 (11) |
RE1—O2vi | 2.417 (10) | RE3—O2xi | 2.590 (11) |
RE1—O3vi | 2.519 (9) | RE3—O3vi | 2.568 (10) |
RE2—O1 | 2.708 (10) | O1—B3 | 1.373 (15) |
RE2—O7 | 2.372 (6) | O2—B2 | 1.360 (13) |
RE2—O5vii | 2.372 (10) | O3—B1 | 1.372 (17) |
RE2—O6vii | 2.594 (8) | O4—B1 | 1.35 (2) |
RE2—O4iv | 2.486 (10) | O5—B1 | 1.355 (16) |
RE2—O1viii | 2.760 (11) | O6—B3 | 1.36 (3) |
RE2—O3vi | 2.897 (10) | O7—B2 | 1.361 (16) |
RE2—O5vi | 2.472 (10) | | |
| | | |
O1i—RE1—O2ii | 79.0 (3) | O1ix—RE3—O6 | 78.8 (4) |
O1i—RE1—O3iii | 67.9 (3) | O2ii—RE3—O6 | 153.6 (2) |
O1i—RE1—O4iii | 75.9 (3) | O1x—RE3—O6 | 78.8 (4) |
O1i—RE1—O5iv | 145.2 (3) | O2xi—RE3—O6 | 153.63 (19) |
O1i—RE1—O4v | 78.8 (3) | O3vi—RE3—O6 | 94.3 (2) |
O1i—RE1—O2vi | 88.3 (3) | O1ix—RE3—O7 | 140.6 (3) |
O1i—RE1—O3vi | 139.2 (3) | O2ii—RE3—O7 | 105.4 (3) |
O2ii—RE1—O3iii | 138.9 (3) | O1x—RE3—O7 | 140.6 (3) |
O2ii—RE1—O4iii | 143.2 (3) | O2xi—RE3—O7 | 105.4 (3) |
O2ii—RE1—O5iv | 129.8 (3) | O3vi—RE3—O7 | 80.8 (2) |
O2ii—RE1—O4v | 78.1 (3) | O1ix—RE3—O2ii | 111.3 (4) |
O2ii—RE1—O2vi | 97.8 (3) | O1ix—RE3—O1x | 57.5 (3) |
O2ii—RE1—O3vi | 62.3 (3) | O1ix—RE3—O2xi | 86.3 (3) |
O3iii—RE1—O4iii | 49.7 (3) | O1ix—RE3—O3vi | 130.2 (3) |
O3iii—RE1—O5iv | 90.4 (3) | O1x—RE3—O2ii | 86.3 (3) |
O3iii—RE1—O4v | 116.5 (3) | O2ii—RE3—O2xi | 52.6 (3) |
O2vi—RE1—O3iii | 59.0 (3) | O2ii—RE3—O3vi | 60.3 (3) |
O3iii—RE1—O3vi | 136.6 (3) | O1x—RE3—O2xi | 111.3 (4) |
O4iii—RE1—O5iv | 69.3 (3) | O1x—RE3—O3vi | 72.7 (3) |
O4iii—RE1—O4v | 70.9 (3) | O2xi—RE3—O3vi | 111.9 (3) |
O2vi—RE1—O4iii | 107.9 (3) | RE2—O1—B3 | 93.3 (12) |
O3vi—RE1—O4iii | 144.2 (3) | RE2—O1—RE2x | 95.1 (3) |
O4v—RE1—O5iv | 87.9 (3) | RE1xii—O1—B3 | 138.8 (12) |
O2vi—RE1—O5iv | 103.9 (3) | RE3vii—O1—B3 | 85.9 (12) |
O3vi—RE1—O5iv | 75.2 (3) | RE2x—O1—B3 | 82.9 (12) |
O2vi—RE1—O4v | 167.0 (3) | RE3viii—O1—B3 | 85.9 (12) |
O3vi—RE1—O4v | 103.9 (3) | RE1iii—O2—B2 | 140.5 (10) |
O2vi—RE1—O3vi | 84.7 (3) | RE3iii—O2—B2 | 91.2 (6) |
O1—RE2—O7 | 102.6 (3) | RE3xiii—O2—B2 | 91.2 (6) |
O1—RE2—O5vii | 85.0 (3) | RE1vi—O2—B2 | 113.0 (10) |
O1—RE2—O6vii | 71.8 (3) | RE1iii—O2—RE1vi | 103.0 (3) |
O1—RE2—O4iv | 148.8 (3) | RE3—O3—B1 | 113.4 (9) |
O1—RE2—O1viii | 120.0 (3) | RE1ii—O3—B1 | 85.8 (10) |
O1—RE2—O3vi | 107.6 (3) | RE1vi—O3—B1 | 144.0 (9) |
O1—RE2—O5vi | 69.3 (3) | RE2vi—O3—B1 | 85.3 (9) |
O5vii—RE2—O7 | 144.8 (4) | RE3vi—O3—B1 | 113.4 (9) |
O6vii—RE2—O7 | 69.8 (3) | RE1ii—O3—RE1vi | 92.3 (3) |
O4iv—RE2—O7 | 107.7 (3) | RE1ii—O4—B1 | 90.4 (8) |
O1viii—RE2—O7 | 76.9 (4) | RE2xiv—O4—B1 | 118.4 (9) |
O3vi—RE2—O7 | 73.8 (3) | RE1xv—O4—B1 | 129.8 (8) |
O5vi—RE2—O7 | 113.9 (4) | RE1ii—O4—RE1xv | 109.1 (3) |
O5vii—RE2—O6vii | 80.6 (3) | RE2ix—O5—B1 | 102.8 (10) |
O4iv—RE2—O5vii | 74.8 (3) | RE1xiv—O5—B1 | 114.6 (9) |
O1viii—RE2—O5vii | 69.8 (3) | RE2vi—O5—B1 | 104.5 (9) |
O3vi—RE2—O5vii | 137.2 (3) | RE2ix—O5—RE2vi | 112.8 (4) |
O5vii—RE2—O5vi | 101.0 (3) | RE3—O6—B3 | 156.6 (14) |
O4iv—RE2—O6vii | 126.2 (3) | RE2ix—O6—B3 | 89.9 (9) |
O1viii—RE2—O6vii | 51.4 (3) | RE2x—O6—B3 | 89.9 (9) |
O3vi—RE2—O6vii | 142.2 (3) | RE3vi—O6—B3 | 156.6 (14) |
O5vi—RE2—O6vii | 140.7 (3) | RE2ix—O6—RE2x | 97.6 (4) |
O1viii—RE2—O4iv | 75.2 (3) | RE2—O7—B2 | 121.0 (4) |
O3vi—RE2—O4iv | 74.5 (3) | RE2—O7—RE2vi | 110.7 (4) |
O4iv—RE2—O5vi | 91.2 (3) | RE3—O7—B2 | 96.8 (11) |
O1viii—RE2—O3vi | 128.3 (3) | RE2vi—O7—B2 | 121.0 (4) |
O1viii—RE2—O5vi | 165.0 (3) | RE3vi—O7—B2 | 96.8 (11) |
O3vi—RE2—O5vi | 51.0 (3) | O3—B1—O4 | 116.7 (10) |
O3—RE3—O6 | 94.3 (2) | O3—B1—O5 | 118.3 (16) |
O3—RE3—O7 | 80.8 (2) | O4—B1—O5 | 123.1 (12) |
O1ix—RE3—O3 | 72.7 (3) | O2—B2—O7 | 116.1 (7) |
O2ii—RE3—O3 | 111.9 (3) | O2—B2—O2vi | 115.1 (14) |
O1x—RE3—O3 | 130.2 (3) | O2vi—B2—O7 | 116.1 (7) |
O2xi—RE3—O3 | 60.3 (3) | O1—B3—O6 | 116.6 (11) |
O3—RE3—O3vi | 156.9 (4) | O1—B3—O1vi | 126 (2) |
O6—RE3—O7 | 74.7 (4) | O1vi—B3—O6 | 116.6 (11) |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, −z+3/2; (iii) x+1/2, −y+1/2, −z+3/2; (iv) −x+1, y−1/2, −z+1; (v) −x+1/2, y−1/2, z+1/2; (vi) x, −y+1/2, z; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Pr2 | b = 15.80592 (6) Å |
Mr = 637.29 | c = 8.67328 (3) Å |
Orthorhombic, Pnma | V = 993.74 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.24883 (3) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 8.33 | Rexp = 2.58 |
Rwp = 12.60 | RBragg = 10.51 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.5245 (2) | 0.08471 (9) | 0.82036 (18) | 1.09 (3) | 0.458 (2) |
RE1 | 0.5245 (2) | 0.08471 (9) | 0.82036 (18) | 1.09 (3) | 0.542 (2) |
Ca2 | 0.6928 (3) | 0.12846 (11) | 0.3469 (2) | 1.09 (3) | 0.6706 (17) |
RE2 | 0.6928 (3) | 0.12846 (11) | 0.3469 (2) | 1.09 (3) | 0.3294 (17) |
Ca3 | 0.3271 (4) | 0.25 | 0.5308 (4) | 1.09 (3) | 0.742 (3) |
RE3 | 0.3271 (4) | 0.25 | 0.5308 (4) | 1.09 (3) | 0.258 (3) |
B1 | 0.345 (4) | 0.4635 (15) | 0.447 (3) | 4.5 | |
B2 | 0.704 (5) | 0.25 | 0.652 (4) | 4.5 | |
B3 | 0.488 (5) | 0.25 | 0.146 (4) | 4.5 | |
O1 | 0.5559 (16) | 0.1787 (6) | 0.0785 (12) | 2.33 (12) | |
O2 | 0.7620 (15) | 0.3251 (6) | 0.7116 (13) | 2.33 (12) | |
O3 | 0.3697 (16) | 0.4097 (7) | 0.5666 (13) | 2.33 (12) | |
O4 | 0.1962 (15) | 0.5119 (7) | 0.4793 (13) | 2.33 (12) | |
O5 | 0.4116 (15) | 0.4657 (6) | 0.3004 (14) | 2.33 (12) | |
O6 | 0.365 (2) | 0.25 | 0.2646 (18) | 2.33 (12) | |
O7 | 0.626 (2) | 0.25 | 0.5092 (19) | 2.33 (12) | |
Geometric parameters (Å, º) top
RE1—O1i | 2.697 (10) | RE3—O3 | 2.562 (11) |
RE1—O2ii | 2.394 (11) | RE3—O6 | 2.325 (16) |
RE1—O3iii | 2.689 (12) | RE3—O7 | 2.175 (15) |
RE1—O4iii | 2.627 (11) | RE3—O1ix | 2.456 (11) |
RE1—O5iv | 2.202 (10) | RE3—O2ii | 2.574 (11) |
RE1—O4v | 2.405 (11) | RE3—O1x | 2.456 (11) |
RE1—O2vi | 2.426 (11) | RE3—O2xi | 2.574 (11) |
RE1—O3vi | 2.472 (11) | RE3—O3vi | 2.562 (11) |
RE2—O1 | 2.652 (11) | O1—B3 | 1.36 (2) |
RE2—O7 | 2.430 (10) | O2—B2 | 1.361 (19) |
RE2—O5vii | 2.522 (11) | O3—B1 | 1.35 (3) |
RE2—O6vii | 2.487 (10) | O4—B1 | 1.35 (3) |
RE2—O4iv | 2.513 (11) | O5—B1 | 1.36 (3) |
RE2—O1viii | 2.824 (12) | O6—B3 | 1.36 (4) |
RE2—O5vi | 2.556 (11) | O7—B2 | 1.36 (4) |
| | | |
O1i—RE1—O2ii | 80.5 (4) | O2xi—RE3—O6 | 152.1 (2) |
O1i—RE1—O3iii | 66.5 (3) | O3vi—RE3—O6 | 96.1 (3) |
O1i—RE1—O4iii | 74.4 (3) | O1ix—RE3—O7 | 139.8 (4) |
O1i—RE1—O5iv | 148.0 (4) | O2ii—RE3—O7 | 104.9 (5) |
O1i—RE1—O4v | 81.0 (4) | O1x—RE3—O7 | 139.8 (4) |
O1i—RE1—O2vi | 86.5 (3) | O2xi—RE3—O7 | 104.9 (5) |
O1i—RE1—O3vi | 139.3 (3) | O3vi—RE3—O7 | 83.7 (3) |
O2ii—RE1—O3iii | 139.7 (3) | O1ix—RE3—O2ii | 113.6 (4) |
O2ii—RE1—O4iii | 143.1 (4) | O1ix—RE3—O1x | 54.6 (3) |
O2ii—RE1—O5iv | 128.4 (4) | O1ix—RE3—O2xi | 88.7 (3) |
O2ii—RE1—O4v | 79.8 (4) | O1ix—RE3—O3vi | 126.5 (4) |
O2ii—RE1—O2vi | 99.7 (3) | O1x—RE3—O2ii | 88.7 (3) |
O2ii—RE1—O3vi | 61.0 (4) | O2ii—RE3—O2xi | 54.9 (3) |
O3iii—RE1—O4iii | 48.5 (3) | O2ii—RE3—O3vi | 57.5 (3) |
O3iii—RE1—O5iv | 90.3 (4) | O1x—RE3—O2xi | 113.6 (4) |
O3iii—RE1—O4v | 115.2 (4) | O1x—RE3—O3vi | 72.0 (3) |
O2vi—RE1—O3iii | 57.5 (4) | O2xi—RE3—O3vi | 111.8 (4) |
O3iii—RE1—O3vi | 138.2 (4) | RE2—O1—B3 | 90.3 (15) |
O4iii—RE1—O5iv | 73.7 (4) | RE2—O1—RE2x | 93.6 (3) |
O4iii—RE1—O4v | 70.0 (4) | RE1xii—O1—B3 | 141.5 (16) |
O2vi—RE1—O4iii | 105.2 (4) | RE3vii—O1—B3 | 94.3 (14) |
O3vi—RE1—O4iii | 145.6 (4) | RE2x—O1—B3 | 78.3 (15) |
O4v—RE1—O5iv | 90.2 (4) | RE3viii—O1—B3 | 94.3 (14) |
O2vi—RE1—O5iv | 99.7 (4) | RE1iii—O2—B2 | 136.1 (17) |
O3vi—RE1—O5iv | 72.7 (4) | RE3iii—O2—B2 | 89.1 (14) |
O2vi—RE1—O4v | 167.4 (4) | RE3xiii—O2—B2 | 89.1 (14) |
O3vi—RE1—O4v | 103.0 (4) | RE1vi—O2—B2 | 116.2 (16) |
O2vi—RE1—O3vi | 87.4 (4) | RE1iii—O2—RE1vi | 105.0 (4) |
O1—RE2—O7 | 101.4 (4) | RE3—O3—B1 | 120.7 (12) |
O1—RE2—O5vii | 88.1 (4) | RE1ii—O3—B1 | 97.8 (13) |
O1—RE2—O6vii | 67.4 (4) | RE1vi—O3—B1 | 136.1 (13) |
O1—RE2—O4iv | 150.0 (3) | RE3vi—O3—B1 | 120.7 (12) |
O1—RE2—O1viii | 117.8 (3) | RE1ii—O3—RE1vi | 95.5 (4) |
O1—RE2—O5vi | 74.8 (4) | RE1ii—O4—B1 | 100.7 (12) |
O5vii—RE2—O7 | 152.3 (4) | RE2xiv—O4—B1 | 106.5 (13) |
O6vii—RE2—O7 | 73.4 (4) | RE1xv—O4—B1 | 133.1 (13) |
O4iv—RE2—O7 | 107.2 (4) | RE1ii—O4—RE1xv | 110.0 (4) |
O1viii—RE2—O7 | 80.3 (4) | RE2ix—O5—B1 | 103.6 (13) |
O5vi—RE2—O7 | 113.1 (4) | RE1xiv—O5—B1 | 122.8 (12) |
O5vii—RE2—O6vii | 86.7 (4) | RE2vi—O5—B1 | 96.9 (13) |
O4iv—RE2—O5vii | 70.7 (4) | RE2ix—O5—RE2vi | 103.8 (4) |
O1viii—RE2—O5vii | 72.3 (3) | RE3—O6—B3 | 145.9 (18) |
O5vii—RE2—O5vi | 94.5 (3) | RE2ix—O6—B3 | 92.0 (11) |
O4iv—RE2—O6vii | 129.7 (4) | RE2x—O6—B3 | 92.0 (11) |
O1viii—RE2—O6vii | 53.4 (4) | RE3vi—O6—B3 | 145.9 (18) |
O5vi—RE2—O6vii | 142.1 (4) | RE2ix—O6—RE2x | 101.2 (5) |
O1viii—RE2—O4iv | 76.7 (3) | RE2—O7—B2 | 116.4 (9) |
O4iv—RE2—O5vi | 85.6 (4) | RE2—O7—RE2vi | 104.5 (6) |
O1viii—RE2—O5vi | 160.6 (3) | RE3—O7—B2 | 109.6 (17) |
O3—RE3—O6 | 96.1 (3) | RE2vi—O7—B2 | 116.4 (9) |
O3—RE3—O7 | 83.7 (3) | RE3vi—O7—B2 | 109.6 (17) |
O1ix—RE3—O3 | 72.0 (3) | O3—B1—O4 | 108 (2) |
O2ii—RE3—O3 | 111.8 (4) | O3—B1—O5 | 133 (2) |
O1x—RE3—O3 | 126.5 (4) | O4—B1—O5 | 118 (2) |
O2xi—RE3—O3 | 57.5 (3) | O2—B2—O7 | 118.3 (14) |
O3—RE3—O3vi | 160.3 (4) | O2—B2—O2vi | 121 (3) |
O6—RE3—O7 | 78.3 (6) | O2vi—B2—O7 | 118.3 (14) |
O1ix—RE3—O6 | 73.2 (4) | O1—B3—O6 | 124.2 (13) |
O2ii—RE3—O6 | 152.1 (2) | O1—B3—O1vi | 112 (3) |
O1x—RE3—O6 | 73.2 (4) | O1vi—B3—O6 | 124.2 (13) |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, −z+3/2; (iii) x+1/2, −y+1/2, −z+3/2; (iv) −x+1, y−1/2, −z+1; (v) −x+1/2, y−1/2, z+1/2; (vi) x, −y+1/2, z; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Nd2 | b = 15.71242 (19) Å |
Mr = 643.95 | c = 8.66674 (11) Å |
Orthorhombic, Pnma | V = 985.72 (2) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.23859 (9) Å | T = 297 K |
Data collection top
PANalytical X'Pert Pro MPD diffractometer | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 2.96 | Rexp = 1.62 |
Rwp = 3.94 | RBragg = 14.5 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.5225 (2) | 0.08399 (9) | 0.82212 (17) | 0.0173 (5) | 0.4798 (16) |
RE1 | 0.5225 (2) | 0.08399 (9) | 0.82212 (17) | 0.0173 (5) | 0.5202 (16) |
Ca2 | 0.6934 (2) | 0.12812 (12) | 0.3447 (2) | 0.0173 (5) | 0.6980 (16) |
RE2 | 0.6934 (2) | 0.12812 (12) | 0.3447 (2) | 0.0173 (5) | 0.3020 (16) |
Ca3 | 0.3271 (4) | 0.25000 | 0.5308 (3) | 0.0173 (5) | 0.645 (3) |
RE3 | 0.3271 (4) | 0.25000 | 0.5308 (3) | 0.0173 (5) | 0.355 (3) |
B1 | 0.312 (2) | 0.4527 (10) | 0.4493 (12) | 0.086 (7) | |
B2 | 0.747 (4) | 0.25000 | 0.6490 (18) | 0.086 (7) | |
B3 | 0.474 (4) | 0.25000 | 0.132 (2) | 0.086 (7) | |
O1 | 0.5494 (13) | 0.1734 (4) | 0.0757 (10) | 0.0331 (14) | |
O2 | 0.7504 (16) | 0.3277 (4) | 0.7244 (10) | 0.0331 (14) | |
O3 | 0.3846 (13) | 0.4034 (6) | 0.5539 (10) | 0.0331 (14) | |
O4 | 0.2111 (12) | 0.5209 (5) | 0.4783 (11) | 0.0331 (14) | |
O5 | 0.3959 (12) | 0.4578 (5) | 0.3089 (9) | 0.0331 (14) | |
O6 | 0.3698 (15) | 0.25000 | 0.2637 (11) | 0.0331 (14) | |
O7 | 0.6490 (16) | 0.25000 | 0.5125 (11) | 0.0331 (14) | |
Geometric parameters (Å, º) top
RE1—O1i | 2.616 (8) | RE3—O3 | 2.454 (9) |
RE1—O2ii | 2.443 (10) | RE3—O6 | 2.335 (10) |
RE1—O3iii | 2.840 (9) | RE3—O7 | 2.336 (12) |
RE1—O4iii | 2.752 (9) | RE3—O1ix | 2.518 (9) |
RE1—O5iv | 2.360 (8) | RE3—O2ii | 2.510 (9) |
RE1—O4v | 2.382 (9) | RE3—O1x | 2.518 (9) |
RE1—O2vi | 2.316 (10) | RE3—O2xi | 2.510 (9) |
RE1—O3vi | 2.538 (9) | RE3—O3vi | 2.454 (9) |
RE2—O1 | 2.651 (9) | O1—B3 | 1.409 (14) |
RE2—O7 | 2.426 (6) | O2—B2 | 1.385 (10) |
RE2—O5vii | 2.397 (8) | O3—B1 | 1.303 (16) |
RE2—O6vii | 2.486 (7) | O4—B1 | 1.321 (17) |
RE2—O4iv | 2.381 (9) | O5—B1 | 1.362 (14) |
RE2—O1viii | 2.761 (9) | O6—B3 | 1.37 (2) |
RE2—O5vi | 2.561 (9) | O7—B2 | 1.38 (2) |
| | | |
O1i—RE1—O2ii | 83.9 (3) | O2xi—RE3—O6 | 150.13 (18) |
O1i—RE1—O3iii | 64.9 (3) | O3vi—RE3—O6 | 93.4 (2) |
O1i—RE1—O4iii | 75.9 (2) | O1ix—RE3—O7 | 140.5 (3) |
O1i—RE1—O5iv | 146.8 (3) | O2ii—RE3—O7 | 106.2 (3) |
O1i—RE1—O4v | 78.4 (3) | O1x—RE3—O7 | 140.5 (3) |
O1i—RE1—O2vi | 86.1 (3) | O2xi—RE3—O7 | 106.2 (3) |
O1i—RE1—O3vi | 139.2 (3) | O3vi—RE3—O7 | 80.6 (2) |
O2ii—RE1—O3iii | 140.1 (3) | O1ix—RE3—O2ii | 111.5 (3) |
O2ii—RE1—O4iii | 147.6 (3) | O1ix—RE3—O1x | 57.1 (2) |
O2ii—RE1—O5iv | 126.8 (3) | O1ix—RE3—O2xi | 84.3 (3) |
O2ii—RE1—O4v | 76.0 (3) | O1ix—RE3—O3vi | 129.4 (3) |
O2ii—RE1—O2vi | 100.0 (3) | O1x—RE3—O2ii | 84.3 (3) |
O2ii—RE1—O3vi | 59.2 (3) | O2ii—RE3—O2xi | 58.2 (2) |
O3iii—RE1—O4iii | 49.2 (3) | O2ii—RE3—O3vi | 59.4 (3) |
O3iii—RE1—O5iv | 90.6 (3) | O1x—RE3—O2xi | 111.5 (3) |
O3iii—RE1—O4v | 118.0 (3) | O1x—RE3—O3vi | 72.3 (3) |
O2vi—RE1—O3iii | 55.9 (3) | O2xi—RE3—O3vi | 116.5 (3) |
O3iii—RE1—O3vi | 134.8 (3) | RE2—O1—B3 | 94.4 (9) |
O4iii—RE1—O5iv | 71.0 (3) | RE2—O1—RE2x | 94.5 (3) |
O4iii—RE1—O4v | 75.3 (3) | RE1xii—O1—B3 | 136.1 (10) |
O2vi—RE1—O4iii | 103.6 (3) | RE3vii—O1—B3 | 91.6 (10) |
O3vi—RE1—O4iii | 144.9 (3) | RE2x—O1—B3 | 76.8 (11) |
O4v—RE1—O5iv | 95.8 (3) | RE3viii—O1—B3 | 91.6 (10) |
O2vi—RE1—O5iv | 98.6 (3) | RE1iii—O2—B2 | 115.9 (12) |
O3vi—RE1—O5iv | 73.9 (3) | RE3iii—O2—B2 | 88.5 (7) |
O2vi—RE1—O4v | 164.3 (3) | RE3xiii—O2—B2 | 88.5 (7) |
O3vi—RE1—O4v | 105.9 (3) | RE1vi—O2—B2 | 133.5 (14) |
O2vi—RE1—O3vi | 84.2 (3) | RE1iii—O2—RE1vi | 107.1 (3) |
O1—RE2—O7 | 105.3 (3) | RE3—O3—B1 | 117.3 (8) |
O1—RE2—O5vii | 84.4 (3) | RE1ii—O3—B1 | 81.4 (7) |
O1—RE2—O6vii | 70.3 (3) | RE1vi—O3—B1 | 138.6 (8) |
O1—RE2—O4iv | 150.5 (3) | RE3vi—O3—B1 | 117.3 (8) |
O1—RE2—O1viii | 121.2 (3) | RE1ii—O3—RE1vi | 90.6 (3) |
O1—RE2—O5vi | 72.8 (3) | RE1ii—O4—B1 | 84.7 (7) |
O5vii—RE2—O7 | 149.2 (3) | RE2xiv—O4—B1 | 122.4 (8) |
O6vii—RE2—O7 | 71.7 (3) | RE1xv—O4—B1 | 128.5 (8) |
O4iv—RE2—O7 | 102.2 (3) | RE1ii—O4—RE1xv | 104.7 (3) |
O1viii—RE2—O7 | 76.7 (3) | RE2ix—O5—B1 | 101.0 (7) |
O5vi—RE2—O7 | 112.2 (3) | RE1xiv—O5—B1 | 126.2 (8) |
O5vii—RE2—O6vii | 84.8 (3) | RE2vi—O5—B1 | 103.6 (7) |
O4iv—RE2—O5vii | 77.4 (3) | RE2ix—O5—RE2vi | 106.5 (3) |
O1viii—RE2—O5vii | 73.3 (3) | RE3—O6—B3 | 154.2 (13) |
O5vii—RE2—O5vi | 98.6 (3) | RE2ix—O6—B3 | 88.2 (8) |
O4iv—RE2—O6vii | 129.8 (3) | RE2x—O6—B3 | 88.2 (8) |
O1viii—RE2—O6vii | 54.3 (3) | RE3vi—O6—B3 | 154.2 (13) |
O5vi—RE2—O6vii | 142.4 (3) | RE2ix—O6—RE2x | 100.8 (4) |
O1viii—RE2—O4iv | 75.5 (3) | RE2—O7—B2 | 116.5 (6) |
O4iv—RE2—O5vi | 87.1 (3) | RE2—O7—RE2vi | 104.3 (4) |
O1viii—RE2—O5vi | 162.0 (2) | RE3—O7—B2 | 117.1 (12) |
O3—RE3—O6 | 93.4 (2) | RE2vi—O7—B2 | 116.5 (6) |
O3—RE3—O7 | 80.6 (2) | RE3vi—O7—B2 | 117.1 (12) |
O1ix—RE3—O3 | 72.3 (3) | O3—B1—O4 | 125.0 (10) |
O2ii—RE3—O3 | 116.5 (3) | O3—B1—O5 | 118.5 (12) |
O1x—RE3—O3 | 129.4 (3) | O4—B1—O5 | 111.6 (11) |
O2xi—RE3—O3 | 59.4 (3) | O2—B2—O7 | 114.4 (11) |
O3—RE3—O3vi | 158.3 (3) | O2—B2—O2vi | 123.7 (12) |
O6—RE3—O7 | 78.5 (4) | O2vi—B2—O7 | 114.4 (11) |
O1ix—RE3—O6 | 75.1 (3) | O1—B3—O6 | 120.2 (8) |
O2ii—RE3—O6 | 150.13 (18) | O1—B3—O1vi | 117.4 (18) |
O1x—RE3—O6 | 75.1 (3) | O1vi—B3—O6 | 120.2 (8) |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, −z+3/2; (iii) x+1/2, −y+1/2, −z+3/2; (iv) −x+1, y−1/2, −z+1; (v) −x+1/2, y−1/2, z+1/2; (vi) x, −y+1/2, z; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Sm2 | b = 15.62415 (7) Å |
Mr = 656.19 | c = 8.64433 (4) Å |
Orthorhombic, Pnma | V = 973.55 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.20829 (3) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 7.33 | Rexp = 2.56 |
Rwp = 10.40 | RBragg = 6.03 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.52113 (17) | 0.08374 (8) | 0.82308 (15) | 1.80 (2) | 0.5246 (15) |
RE1 | 0.52113 (17) | 0.08374 (8) | 0.82308 (15) | 1.80 (2) | 0.4754 (15) |
Ca2 | 0.6938 (2) | 0.12747 (10) | 0.34442 (19) | 1.80 (2) | 0.7157 (12) |
RE2 | 0.6938 (2) | 0.12747 (10) | 0.34442 (19) | 1.80 (2) | 0.2843 (12) |
Ca3 | 0.3266 (2) | 0.25 | 0.5328 (2) | 1.80 (2) | 0.519 (2) |
RE3 | 0.3266 (2) | 0.25 | 0.5328 (2) | 1.80 (2) | 0.481 (2) |
B1 | 0.328 (3) | 0.4558 (13) | 0.451 (3) | 6.0 (5) | |
B2 | 0.716 (4) | 0.25 | 0.658 (4) | 6.0 (5) | |
B3 | 0.491 (4) | 0.25 | 0.138 (3) | 6.0 (5) | |
O1 | 0.5547 (13) | 0.1767 (5) | 0.0714 (10) | 4.52 (11) | |
O2 | 0.7503 (14) | 0.3280 (5) | 0.7203 (10) | 4.52 (11) | |
O3 | 0.4031 (13) | 0.4025 (6) | 0.5571 (12) | 4.52 (11) | |
O4 | 0.2029 (13) | 0.5168 (6) | 0.4909 (11) | 4.52 (11) | |
O5 | 0.4013 (13) | 0.4591 (6) | 0.3059 (12) | 4.52 (11) | |
O6 | 0.3813 (18) | 0.25 | 0.2660 (15) | 4.52 (11) | |
O7 | 0.6575 (18) | 0.25 | 0.5084 (15) | 4.52 (11) | |
Geometric parameters (Å, º) top
RE1—O1i | 2.603 (9) | RE3—O3 | 2.455 (9) |
RE1—O2ii | 2.419 (9) | RE3—O6 | 2.340 (13) |
RE1—O4iii | 2.602 (10) | RE3—O7 | 2.395 (13) |
RE1—O5iv | 2.313 (10) | RE3—O1ix | 2.442 (9) |
RE1—O4v | 2.410 (9) | RE3—O2ii | 2.519 (9) |
RE1—O2vi | 2.328 (9) | RE3—O1x | 2.442 (9) |
RE1—O3vi | 2.461 (10) | RE3—O2xi | 2.519 (9) |
RE2—O1 | 2.677 (9) | RE3—O3vi | 2.455 (9) |
RE2—O7 | 2.396 (8) | O1—B3 | 1.362 (17) |
RE2—O5vii | 2.399 (10) | O2—B2 | 1.355 (16) |
RE2—O6vii | 2.530 (9) | O3—B1 | 1.35 (3) |
RE2—O4iv | 2.360 (10) | O4—B1 | 1.36 (2) |
RE2—O1viii | 2.809 (9) | O5—B1 | 1.36 (3) |
RE2—O3vi | 2.827 (10) | O6—B3 | 1.36 (3) |
RE2—O5vi | 2.527 (9) | O7—B2 | 1.36 (4) |
| | | |
O1i—RE1—O2ii | 83.4 (3) | O2xi—RE3—O6 | 150.71 (19) |
O1i—RE1—O4iii | 77.3 (3) | O3vi—RE3—O6 | 92.7 (3) |
O1i—RE1—O5iv | 147.7 (3) | O1ix—RE3—O7 | 140.1 (3) |
O1i—RE1—O4v | 78.9 (3) | O2ii—RE3—O7 | 107.0 (4) |
O1i—RE1—O2vi | 85.3 (3) | O1x—RE3—O7 | 140.1 (3) |
O1i—RE1—O3vi | 138.9 (3) | O2xi—RE3—O7 | 107.0 (4) |
O2ii—RE1—O4iii | 147.8 (3) | O3vi—RE3—O7 | 77.5 (2) |
O2ii—RE1—O5iv | 126.9 (3) | O1ix—RE3—O2ii | 111.4 (3) |
O2ii—RE1—O4v | 78.5 (3) | O1ix—RE3—O1x | 55.9 (3) |
O2ii—RE1—O2vi | 100.1 (3) | O1ix—RE3—O2xi | 84.9 (3) |
O2ii—RE1—O3vi | 61.7 (3) | O1ix—RE3—O3vi | 131.8 (3) |
O4iii—RE1—O5iv | 70.6 (3) | O1x—RE3—O2ii | 84.9 (3) |
O4iii—RE1—O4v | 72.7 (3) | O2ii—RE3—O2xi | 57.9 (3) |
O2vi—RE1—O4iii | 103.7 (3) | O2ii—RE3—O3vi | 60.5 (3) |
O3vi—RE1—O4iii | 143.5 (3) | O1x—RE3—O2xi | 111.4 (3) |
O4v—RE1—O5iv | 95.0 (3) | O1x—RE3—O3vi | 75.9 (3) |
O2vi—RE1—O5iv | 98.2 (3) | O2xi—RE3—O3vi | 116.5 (3) |
O3vi—RE1—O5iv | 73.0 (3) | RE2—O1—B3 | 89.7 (11) |
O2vi—RE1—O4v | 164.2 (3) | RE2—O1—RE2x | 92.3 (3) |
O3vi—RE1—O4v | 111.6 (3) | RE1xii—O1—B3 | 141.9 (12) |
O2vi—RE1—O3vi | 80.6 (3) | RE3vii—O1—B3 | 91.8 (11) |
O1—RE2—O7 | 104.5 (3) | RE2x—O1—B3 | 79.0 (12) |
O1—RE2—O5vii | 85.3 (3) | RE3viii—O1—B3 | 91.8 (11) |
O1—RE2—O6vii | 69.5 (3) | RE1iii—O2—B2 | 126.7 (14) |
O1—RE2—O4iv | 149.4 (3) | RE3iii—O2—B2 | 86.6 (14) |
O1—RE2—O1viii | 119.8 (3) | RE3xiii—O2—B2 | 86.6 (14) |
O1—RE2—O3vi | 110.1 (3) | RE1vi—O2—B2 | 123.7 (14) |
O1—RE2—O5vi | 74.1 (3) | RE1iii—O2—RE1vi | 107.1 (3) |
O5vii—RE2—O7 | 147.0 (4) | RE3—O3—B1 | 116.7 (11) |
O6vii—RE2—O7 | 71.2 (4) | RE1vi—O3—B1 | 135.9 (11) |
O4iv—RE2—O7 | 105.2 (4) | RE2vi—O3—B1 | 87.6 (11) |
O1viii—RE2—O7 | 74.3 (4) | RE3vi—O3—B1 | 116.7 (11) |
O3vi—RE2—O7 | 70.5 (3) | RE1ii—O4—B1 | 93.9 (11) |
O5vi—RE2—O7 | 114.5 (4) | RE2xiv—O4—B1 | 117.3 (11) |
O5vii—RE2—O6vii | 83.6 (3) | RE1xv—O4—B1 | 126.7 (12) |
O4iv—RE2—O5vii | 73.6 (3) | RE1ii—O4—RE1xv | 107.3 (3) |
O1viii—RE2—O5vii | 73.6 (3) | RE2ix—O5—B1 | 103.6 (10) |
O3vi—RE2—O5vii | 136.1 (3) | RE1xiv—O5—B1 | 124.7 (10) |
O5vii—RE2—O5vi | 98.5 (3) | RE2vi—O5—B1 | 100.5 (10) |
O4iv—RE2—O6vii | 127.8 (4) | RE2ix—O5—RE2vi | 106.9 (4) |
O1viii—RE2—O6vii | 52.8 (3) | RE3—O6—B3 | 154.2 (14) |
O3vi—RE2—O6vii | 140.1 (3) | RE2ix—O6—B3 | 90.2 (9) |
O5vi—RE2—O6vii | 143.2 (4) | RE2x—O6—B3 | 90.2 (9) |
O1viii—RE2—O4iv | 75.7 (3) | RE3vi—O6—B3 | 154.2 (14) |
O3vi—RE2—O4iv | 73.8 (3) | RE2ix—O6—RE2x | 98.3 (4) |
O4iv—RE2—O5vi | 87.2 (3) | RE2—O7—B2 | 121.9 (6) |
O1viii—RE2—O3vi | 124.3 (3) | RE2—O7—RE2vi | 106.1 (5) |
O1viii—RE2—O5vi | 162.5 (3) | RE3—O7—B2 | 103.0 (14) |
O3vi—RE2—O5vi | 51.6 (3) | RE2vi—O7—B2 | 121.9 (6) |
O3—RE3—O6 | 92.7 (3) | RE3vi—O7—B2 | 103.0 (14) |
O3—RE3—O7 | 77.5 (2) | O3—B1—O4 | 122 (2) |
O1ix—RE3—O3 | 75.9 (3) | O3—B1—O5 | 119.5 (17) |
O2ii—RE3—O3 | 116.5 (3) | O4—B1—O5 | 117.7 (18) |
O1x—RE3—O3 | 131.8 (3) | O2—B2—O7 | 115.8 (14) |
O2xi—RE3—O3 | 60.5 (3) | O2—B2—O2vi | 128 (3) |
O3—RE3—O3vi | 152.2 (3) | O2vi—B2—O7 | 115.8 (14) |
O6—RE3—O7 | 75.2 (4) | O1—B3—O6 | 122.7 (10) |
O1ix—RE3—O6 | 76.8 (3) | O1—B3—O1vi | 115 (2) |
O2ii—RE3—O6 | 150.71 (19) | O1vi—B3—O6 | 122.7 (10) |
O1x—RE3—O6 | 76.8 (3) | | |
Symmetry codes: (i) x, y, z+1; (ii) x−1/2, −y+1/2, −z+3/2; (iii) x+1/2, −y+1/2, −z+3/2; (iv) −x+1, y−1/2, −z+1; (v) −x+1/2, y−1/2, z+1/2; (vi) x, −y+1/2, z; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Gd2 | b = 15.54488 (2) Å |
Mr = 669.97 | c = 8.619761 (13) Å |
Orthorhombic, Pnma | V = 963.89 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.193564 (11) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 6.28 | Rexp = 2.76 |
Rwp = 8.59 | RBragg = 6.92 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.52003 (12) | 0.08355 (6) | 0.82322 (11) | 1.506 (16) | 0.5336 (11) |
RE1 | 0.52003 (12) | 0.08355 (6) | 0.82322 (11) | 1.506 (16) | 0.4664 (11) |
Ca2 | 0.69617 (17) | 0.12722 (7) | 0.34254 (15) | 1.506 (16) | 0.7570 (9) |
RE2 | 0.69617 (17) | 0.12722 (7) | 0.34254 (15) | 1.506 (16) | 0.2430 (9) |
Ca3 | 0.32683 (15) | 0.25 | 0.53309 (13) | 1.506 (16) | 0.4189 (15) |
RE3 | 0.32683 (15) | 0.25 | 0.53309 (13) | 1.506 (16) | 0.5811 (15) |
B1 | 0.329 (2) | 0.4556 (10) | 0.4511 (18) | 4.5 (3) | |
B2 | 0.704 (3) | 0.25 | 0.659 (3) | 4.5 (3) | |
B3 | 0.494 (3) | 0.25 | 0.138 (2) | 4.5 (3) | |
O1 | 0.5512 (10) | 0.1755 (4) | 0.0702 (8) | 3.96 (8) | |
O2 | 0.7499 (10) | 0.3272 (4) | 0.7227 (8) | 3.96 (8) | |
O3 | 0.3938 (10) | 0.3999 (4) | 0.5588 (9) | 3.96 (8) | |
O4 | 0.2008 (10) | 0.5172 (4) | 0.4822 (8) | 3.96 (8) | |
O5 | 0.4013 (10) | 0.4566 (4) | 0.3056 (9) | 3.96 (8) | |
O6 | 0.3861 (14) | 0.25 | 0.2679 (12) | 3.96 (8) | |
O7 | 0.6555 (14) | 0.25 | 0.5069 (11) | 3.96 (8) | |
Geometric parameters (Å, º) top
RE1—O3i | 2.467 (8) | RE3—O3 | 2.390 (6) |
RE1—O1ii | 2.574 (7) | RE3—O6 | 2.325 (10) |
RE1—O2iii | 2.420 (7) | RE3—O7 | 2.375 (10) |
RE1—O4iv | 2.638 (7) | RE3—O1ix | 2.463 (7) |
RE1—O5v | 2.334 (7) | RE3—O2iii | 2.486 (7) |
RE1—O4vi | 2.338 (7) | RE3—O1x | 2.463 (7) |
RE1—O2i | 2.326 (7) | RE3—O2xi | 2.486 (7) |
RE2—O1 | 2.676 (7) | O1—B3 | 1.361 (12) |
RE2—O7 | 2.395 (6) | O2—B2 | 1.360 (13) |
RE2—O5vii | 2.346 (7) | O3—B1 | 1.352 (17) |
RE2—O6vii | 2.533 (7) | O4—B1 | 1.356 (16) |
RE2—O4v | 2.399 (7) | O5—B1 | 1.358 (17) |
RE2—O1viii | 2.766 (7) | O6—B3 | 1.36 (2) |
RE2—O5i | 2.510 (7) | O7—B2 | 1.36 (3) |
RE3—O3i | 2.390 (6) | | |
| | | |
O1ii—RE1—O4vi | 79.6 (2) | O1x—RE3—O2xi | 110.7 (2) |
O1ii—RE1—O2i | 85.1 (2) | O1x—RE3—O3i | 74.8 (2) |
O1ii—RE1—O3i | 137.6 (2) | O2xi—RE3—O3i | 115.9 (2) |
O2iii—RE1—O4iv | 147.2 (2) | O1ix—RE3—O7 | 140.1 (2) |
O2iii—RE1—O5v | 127.0 (2) | O2iii—RE3—O7 | 107.6 (3) |
O2iii—RE1—O4vi | 78.7 (2) | O1x—RE3—O7 | 140.1 (2) |
O2iii—RE1—O2i | 99.7 (2) | O2xi—RE3—O7 | 107.6 (3) |
O2iii—RE1—O3i | 59.6 (2) | O3—RE3—O6 | 93.11 (19) |
O4iv—RE1—O5v | 71.4 (2) | O3—RE3—O7 | 78.94 (18) |
O4iv—RE1—O4vi | 72.6 (2) | O1ix—RE3—O3 | 74.8 (2) |
O2i—RE1—O4iv | 103.9 (2) | O2iii—RE3—O3 | 115.9 (2) |
O3i—RE1—O4iv | 146.2 (2) | O1x—RE3—O3 | 130.9 (2) |
O4vi—RE1—O5v | 94.1 (2) | O2xi—RE3—O3 | 59.7 (2) |
O2i—RE1—O5v | 98.9 (2) | O3—RE3—O3i | 154.4 (3) |
O3i—RE1—O5v | 74.8 (2) | RE2—O1—B3 | 88.8 (8) |
O2i—RE1—O4vi | 164.7 (2) | RE2—O1—RE2x | 92.6 (2) |
O3i—RE1—O4vi | 109.7 (2) | RE1xii—O1—B3 | 143.3 (9) |
O2i—RE1—O3i | 81.7 (2) | RE3vii—O1—B3 | 89.9 (8) |
O1ii—RE1—O2iii | 83.5 (2) | RE2x—O1—B3 | 80.5 (9) |
O1ii—RE1—O4iv | 76.2 (2) | RE3viii—O1—B3 | 89.9 (8) |
O1ii—RE1—O5v | 147.3 (2) | RE3iv—O2—B2 | 88.3 (10) |
O1—RE2—O7 | 104.4 (2) | RE1iv—O2—B2 | 129.4 (11) |
O1—RE2—O5vii | 85.6 (2) | RE3xiii—O2—B2 | 88.3 (10) |
O1—RE2—O6vii | 70.7 (3) | RE1i—O2—B2 | 120.3 (10) |
O5vii—RE2—O7 | 147.3 (3) | RE1iv—O2—RE1i | 106.9 (2) |
O6vii—RE2—O7 | 71.8 (3) | RE3—O3—B1 | 119.4 (8) |
O4v—RE2—O7 | 103.5 (3) | RE3i—O3—B1 | 119.4 (8) |
O1viii—RE2—O7 | 74.7 (3) | RE1i—O3—B1 | 134.0 (8) |
O1—RE2—O4v | 150.8 (2) | RE1iii—O4—B1 | 92.4 (7) |
O1—RE2—O1viii | 121.5 (2) | RE2xiv—O4—B1 | 114.7 (8) |
O1—RE2—O5i | 72.8 (2) | RE1xv—O4—B1 | 131.1 (8) |
O5vii—RE2—O5i | 100.0 (2) | RE1iii—O4—RE1xv | 107.4 (3) |
O4v—RE2—O6vii | 127.4 (3) | RE2ix—O5—B1 | 104.8 (7) |
O1viii—RE2—O6vii | 53.1 (3) | RE1xiv—O5—B1 | 122.8 (8) |
O5i—RE2—O6vii | 143.1 (3) | RE2i—O5—B1 | 101.6 (7) |
O1viii—RE2—O4v | 74.8 (2) | RE2ix—O5—RE2i | 108.2 (3) |
O4v—RE2—O5i | 88.3 (2) | RE3—O6—B3 | 155.8 (11) |
O1viii—RE2—O5i | 162.9 (2) | RE2ix—O6—B3 | 89.9 (7) |
O5vii—RE2—O6vii | 82.8 (2) | RE2x—O6—B3 | 89.9 (7) |
O4v—RE2—O5vii | 75.7 (2) | RE3i—O6—B3 | 155.8 (11) |
O1viii—RE2—O5vii | 73.6 (2) | RE2ix—O6—RE2x | 97.8 (3) |
O5i—RE2—O7 | 112.7 (3) | RE3—O7—B2 | 99.5 (11) |
O2xi—RE3—O6 | 150.86 (15) | RE2—O7—B2 | 122.7 (4) |
O3i—RE3—O6 | 93.11 (19) | RE2—O7—RE2i | 105.7 (4) |
O1x—RE3—O6 | 78.0 (3) | RE3i—O7—B2 | 99.5 (11) |
O6—RE3—O7 | 74.0 (3) | RE2i—O7—B2 | 122.7 (4) |
O1ix—RE3—O6 | 78.0 (3) | O3—B1—O4 | 123.4 (12) |
O2iii—RE3—O6 | 150.86 (15) | O3—B1—O5 | 120.6 (12) |
O3i—RE3—O7 | 78.94 (18) | O4—B1—O5 | 115.8 (12) |
O1ix—RE3—O2iii | 110.7 (2) | O2—B2—O7 | 116.9 (10) |
O1ix—RE3—O1x | 56.1 (2) | O2—B2—O2i | 123.8 (19) |
O1ix—RE3—O2xi | 84.3 (2) | O2i—B2—O7 | 116.9 (10) |
O1ix—RE3—O3i | 130.9 (2) | O1—B3—O6 | 121.7 (7) |
O1x—RE3—O2iii | 84.3 (2) | O1—B3—O1i | 116.6 (14) |
O2iii—RE3—O2xi | 57.7 (2) | O1i—B3—O6 | 121.7 (7) |
O2iii—RE3—O3i | 59.7 (2) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Tb2 | b = 15.54541 (8) Å |
Mr = 673.32 | c = 8.60357 (5) Å |
Orthorhombic, Pnma | V = 960.19 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.17921 (4) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 5.89 | Rexp = 2.42 |
Rwp = 8.33 | RBragg = 4.70 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.51968 (15) | 0.08342 (7) | 0.82240 (14) | 1.86 (2) | 0.5458 (12) |
RE1 | 0.51968 (15) | 0.08342 (7) | 0.82240 (14) | 1.86 (2) | 0.4542 (12) |
Ca2 | 0.6968 (2) | 0.12680 (8) | 0.34285 (17) | 1.86 (2) | 0.7396 (9) |
RE2 | 0.6968 (2) | 0.12680 (8) | 0.34285 (17) | 1.86 (2) | 0.2604 (9) |
Ca3 | 0.32600 (19) | 0.25 | 0.53300 (16) | 1.86 (2) | 0.4291 (15) |
RE3 | 0.32600 (19) | 0.25 | 0.53300 (16) | 1.86 (2) | 0.5709 (15) |
B1 | 0.338 (3) | 0.4615 (11) | 0.452 (2) | 4.5 (4) | |
B2 | 0.713 (3) | 0.25 | 0.661 (3) | 4.5 (4) | |
B3 | 0.491 (4) | 0.25 | 0.139 (3) | 4.5 (4) | |
O1 | 0.5465 (11) | 0.1765 (4) | 0.0675 (9) | 4.49 (10) | |
O2 | 0.7538 (12) | 0.3270 (4) | 0.7234 (9) | 4.49 (10) | |
O3 | 0.3866 (12) | 0.3987 (5) | 0.5460 (11) | 4.49 (10) | |
O4 | 0.2093 (11) | 0.5194 (5) | 0.4858 (9) | 4.49 (10) | |
O5 | 0.4036 (12) | 0.4540 (5) | 0.3058 (11) | 4.49 (10) | |
O6 | 0.3737 (16) | 0.25 | 0.2641 (13) | 4.49 (10) | |
O7 | 0.6594 (16) | 0.25 | 0.5104 (13) | 4.49 (10) | |
Geometric parameters (Å, º) top
RE1—O3i | 2.578 (9) | RE3—O3 | 2.355 (8) |
RE1—O1ii | 2.565 (7) | RE3—O6 | 2.339 (11) |
RE1—O2iii | 2.395 (8) | RE3—O7 | 2.401 (12) |
RE1—O4iv | 2.670 (8) | RE3—O1ix | 2.466 (8) |
RE1—O5v | 2.360 (8) | RE3—O2iii | 2.469 (8) |
RE1—O4vi | 2.381 (8) | RE3—O1x | 2.466 (8) |
RE1—O2i | 2.343 (8) | RE3—O2xi | 2.469 (8) |
RE2—O1 | 2.715 (8) | O1—B3 | 1.358 (16) |
RE2—O7 | 2.412 (7) | O2—B2 | 1.344 (13) |
RE2—O5vii | 2.328 (9) | O3—B1 | 1.315 (19) |
RE2—O6vii | 2.475 (7) | O4—B1 | 1.32 (2) |
RE2—O4v | 2.327 (8) | O5—B1 | 1.35 (2) |
RE2—O1viii | 2.738 (8) | O6—B3 | 1.37 (3) |
RE2—O5i | 2.472 (9) | O7—B2 | 1.35 (3) |
RE3—O3i | 2.355 (8) | | |
| | | |
O1ii—RE1—O4vi | 78.6 (3) | O1x—RE3—O2xi | 110.6 (3) |
O1ii—RE1—O2i | 84.8 (2) | O1x—RE3—O3i | 73.3 (3) |
O1ii—RE1—O3i | 136.5 (2) | O2xi—RE3—O3i | 118.3 (3) |
O2iii—RE1—O4iv | 148.9 (3) | O1ix—RE3—O7 | 141.5 (2) |
O2iii—RE1—O5v | 127.2 (3) | O2iii—RE3—O7 | 106.1 (3) |
O2iii—RE1—O4vi | 77.9 (3) | O1x—RE3—O7 | 141.5 (2) |
O2iii—RE1—O2i | 99.6 (3) | O2xi—RE3—O7 | 106.1 (3) |
O2iii—RE1—O3i | 59.4 (3) | O3—RE3—O6 | 91.1 (2) |
O4iv—RE1—O5v | 70.1 (3) | O3—RE3—O7 | 79.6 (2) |
O4iv—RE1—O4vi | 74.8 (3) | O1ix—RE3—O3 | 73.3 (3) |
O2i—RE1—O4iv | 102.4 (3) | O2iii—RE3—O3 | 118.3 (3) |
O3i—RE1—O4iv | 145.4 (2) | O1x—RE3—O3 | 128.5 (3) |
O4vi—RE1—O5v | 94.6 (3) | O2xi—RE3—O3 | 61.5 (3) |
O2i—RE1—O5v | 99.8 (3) | O3—RE3—O3i | 158.0 (3) |
O3i—RE1—O5v | 75.4 (3) | RE2—O1—B3 | 87.8 (11) |
O2i—RE1—O4vi | 163.4 (3) | RE2—O1—RE2x | 92.2 (2) |
O3i—RE1—O4vi | 109.5 (3) | RE1xii—O1—B3 | 145.6 (12) |
O2i—RE1—O3i | 82.3 (3) | RE3vii—O1—B3 | 90.4 (11) |
O1ii—RE1—O2iii | 82.4 (2) | RE2x—O1—B3 | 80.8 (12) |
O1ii—RE1—O4iv | 78.0 (2) | RE3viii—O1—B3 | 90.4 (11) |
O1ii—RE1—O5v | 148.0 (3) | RE3iv—O2—B2 | 87.3 (10) |
O1—RE2—O7 | 104.6 (3) | RE1iv—O2—B2 | 128.7 (11) |
O1—RE2—O5vii | 85.9 (3) | RE3xiii—O2—B2 | 87.3 (10) |
O1—RE2—O6vii | 70.1 (3) | RE1i—O2—B2 | 121.2 (10) |
O5vii—RE2—O7 | 145.9 (3) | RE1iv—O2—RE1i | 106.6 (2) |
O6vii—RE2—O7 | 70.4 (3) | RE3—O3—B1 | 130.6 (10) |
O4v—RE2—O7 | 102.9 (3) | RE3i—O3—B1 | 130.6 (10) |
O1viii—RE2—O7 | 73.1 (3) | RE1i—O3—B1 | 125.9 (9) |
O1—RE2—O4v | 150.7 (2) | RE1iii—O4—B1 | 94.9 (9) |
O1—RE2—O1viii | 122.0 (2) | RE2xiv—O4—B1 | 115.2 (9) |
O1—RE2—O5i | 72.2 (3) | RE1xv—O4—B1 | 129.6 (9) |
O5vii—RE2—O5i | 101.4 (3) | RE1iii—O4—RE1xv | 105.3 (3) |
O4v—RE2—O6vii | 129.9 (3) | RE2ix—O5—B1 | 109.7 (10) |
O1viii—RE2—O6vii | 54.3 (3) | RE1xiv—O5—B1 | 116.4 (9) |
O5i—RE2—O6vii | 141.5 (3) | RE2i—O5—B1 | 102.8 (10) |
O1viii—RE2—O4v | 76.0 (2) | RE2ix—O5—RE2i | 109.9 (3) |
O4v—RE2—O5i | 87.9 (3) | RE3—O6—B3 | 150.4 (14) |
O1viii—RE2—O5i | 163.9 (2) | RE2ix—O6—B3 | 91.3 (8) |
O5vii—RE2—O6vii | 83.5 (3) | RE2x—O6—B3 | 91.3 (8) |
O4v—RE2—O5vii | 77.1 (3) | RE3i—O6—B3 | 150.4 (14) |
O1viii—RE2—O5vii | 73.9 (3) | RE2ix—O6—RE2x | 101.4 (4) |
O5i—RE2—O7 | 112.7 (3) | RE3—O7—B2 | 101.9 (11) |
O2xi—RE3—O6 | 150.53 (16) | RE2—O7—B2 | 122.8 (4) |
O3i—RE3—O6 | 91.1 (2) | RE2—O7—RE2i | 105.1 (4) |
O1x—RE3—O6 | 76.8 (3) | RE3i—O7—B2 | 101.9 (11) |
O6—RE3—O7 | 76.9 (4) | RE2i—O7—B2 | 122.8 (4) |
O1ix—RE3—O6 | 76.8 (3) | O3—B1—O4 | 123.8 (15) |
O2iii—RE3—O6 | 150.53 (16) | O3—B1—O5 | 114.6 (14) |
O3i—RE3—O7 | 79.6 (2) | O4—B1—O5 | 120.5 (14) |
O1ix—RE3—O2iii | 110.6 (3) | O2—B2—O7 | 116.4 (11) |
O1ix—RE3—O1x | 55.2 (2) | O2—B2—O2i | 125.9 (19) |
O1ix—RE3—O2xi | 84.4 (3) | O2i—B2—O7 | 116.4 (11) |
O1ix—RE3—O3i | 128.5 (3) | O1—B3—O6 | 122.5 (10) |
O1x—RE3—O2iii | 84.4 (3) | O1—B3—O1i | 114.6 (19) |
O2iii—RE3—O2xi | 58.0 (2) | O1i—B3—O6 | 122.5 (10) |
O2iii—RE3—O3i | 61.5 (3) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Dy2 | b = 15.4898 (3) Å |
Mr = 680.47 | c = 8.58047 (16) Å |
Orthorhombic, Pnma | V = 951.56 (3) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.15939 (13) Å | T = 297 K |
Data collection top
PANalytical X'Pert Pro MPD diffractometer | 2θmin = 0.502°, 2θmax = 40.00° |
Refinement top
Rp = 1.99 | Rexp = 1.39 |
Rwp = 2.94 | RBragg = 12.3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ca1 | 0.5163 (5) | 0.0824 (2) | 0.8242 (4) | 0.0064 (11) | 0.558 (3) |
RE1 | 0.5163 (5) | 0.0824 (2) | 0.8242 (4) | 0.0064 (11) | 0.442 (3) |
Ca2 | 0.6993 (6) | 0.1286 (3) | 0.3400 (5) | 0.0064 (11) | 0.766 (4) |
RE2 | 0.6993 (6) | 0.1286 (3) | 0.3400 (5) | 0.0064 (11) | 0.234 (4) |
Ca3 | 0.3272 (5) | 0.25000 | 0.5348 (4) | 0.0064 (11) | 0.352 (5) |
RE3 | 0.3272 (5) | 0.25000 | 0.5348 (4) | 0.0064 (11) | 0.648 (5) |
B1 | 0.285 (2) | 0.4510 (9) | 0.4442 (11) | 0.05699 | |
B2 | 0.798 (2) | 0.25000 | 0.6659 (17) | 0.05699 | |
B3 | 0.486 (7) | 0.25000 | 0.140 (5) | 0.05699 | |
O1 | 0.561 (2) | 0.1762 (7) | 0.077 (2) | 0.037 (3) | |
O2 | 0.752 (3) | 0.3267 (7) | 0.7367 (17) | 0.037 (3) | |
O3 | 0.360 (2) | 0.4141 (11) | 0.5751 (15) | 0.037 (3) | |
O4 | 0.194 (2) | 0.5242 (7) | 0.489 (2) | 0.037 (3) | |
O5 | 0.389 (2) | 0.4698 (11) | 0.3136 (15) | 0.037 (3) | |
O6 | 0.359 (3) | 0.25000 | 0.259 (2) | 0.037 (3) | |
O7 | 0.671 (3) | 0.25000 | 0.546 (2) | 0.037 (3) | |
Geometric parameters (Å, º) top
RE1—O2i | 2.322 (18) | RE3—O6 | 2.377 (18) |
RE1—O3i | 2.413 (14) | RE3—O7 | 2.46 (2) |
RE1—O1ii | 2.630 (16) | RE3—O1ix | 2.421 (14) |
RE1—O2iii | 2.416 (19) | RE3—O2iii | 2.355 (14) |
RE1—O3iv | 2.609 (15) | RE3—B2iii | 2.577 (15) |
RE1—O4iv | 2.630 (15) | RE3—O1x | 2.421 (14) |
RE1—O5v | 2.214 (16) | RE3—O2xi | 2.355 (14) |
RE1—O4vi | 2.254 (15) | RE3—O3i | 2.576 (17) |
RE2—O5i | 2.704 (16) | O1—B3 | 1.37 (3) |
RE2—O1 | 2.572 (17) | O2—B2 | 1.374 (14) |
RE2—O7 | 2.589 (13) | O3—B1 | 1.370 (18) |
RE2—O5vii | 2.430 (16) | O4—B1 | 1.363 (18) |
RE2—O6vii | 2.359 (13) | O5—B1 | 1.377 (18) |
RE2—O4v | 2.313 (15) | O6—B3 | 1.37 (5) |
RE2—O1viii | 2.785 (15) | O7—B2 | 1.37 (2) |
RE3—O3 | 2.576 (17) | | |
| | | |
O2i—RE1—O3i | 92.1 (6) | O3—RE3—B2iii | 82.7 (3) |
O2iii—RE1—O2i | 98.4 (6) | O1x—RE3—O3 | 126.2 (4) |
O2iii—RE1—O3i | 55.4 (5) | O2xi—RE3—O3 | 53.9 (4) |
O3iv—RE1—O4iv | 49.8 (5) | O3—RE3—O3i | 161.3 (5) |
O3iv—RE1—O5v | 84.5 (5) | O6—RE3—O7 | 86.7 (7) |
O1ii—RE1—O2iii | 87.2 (5) | O1ix—RE3—O6 | 71.4 (6) |
O1ii—RE1—O3iv | 66.5 (5) | O2iii—RE3—O6 | 148.3 (3) |
O1ii—RE1—O4iv | 77.6 (4) | O6—RE3—B2iii | 179.2 (6) |
O1ii—RE1—O5v | 147.0 (5) | O1x—RE3—O6 | 71.4 (6) |
O1ii—RE1—O4vi | 77.6 (5) | O2xi—RE3—O6 | 148.3 (3) |
O1ii—RE1—O2i | 81.0 (5) | O3i—RE3—O6 | 97.2 (3) |
O1ii—RE1—O3i | 140.8 (5) | O1ix—RE3—O7 | 143.3 (4) |
O2iii—RE1—O3iv | 143.0 (5) | O2iii—RE3—O7 | 101.3 (6) |
O2iii—RE1—O4iv | 151.3 (5) | O7—RE3—B2iii | 92.4 (5) |
O2iii—RE1—O5v | 125.7 (5) | O1x—RE3—O7 | 143.3 (4) |
O2iii—RE1—O4vi | 81.1 (5) | O2xi—RE3—O7 | 101.3 (6) |
O3i—RE1—O4vi | 104.8 (6) | O3i—RE3—O7 | 84.5 (3) |
O4iv—RE1—O4vi | 71.9 (5) | O1ix—RE3—O2iii | 112.8 (6) |
O2i—RE1—O4iv | 103.1 (5) | RE2—O1—B3 | 92.5 (19) |
O3i—RE1—O4iv | 141.1 (5) | RE2—O1—RE2x | 93.3 (5) |
O3iv—RE1—O4vi | 115.5 (5) | RE1xii—O1—B3 | 137 (2) |
O2i—RE1—O3iv | 53.8 (5) | RE3vii—O1—B3 | 94.1 (18) |
O3iv—RE1—O3i | 136.9 (5) | RE2x—O1—B3 | 75.9 (19) |
O4iv—RE1—O5v | 71.5 (5) | RE3viii—O1—B3 | 94.1 (18) |
O4vi—RE1—O5v | 103.0 (5) | RE3iv—O2—B2 | 82.9 (8) |
O2i—RE1—O5v | 94.7 (5) | RE1iv—O2—B2 | 102.7 (12) |
O3i—RE1—O5v | 71.7 (5) | RE3xiii—O2—B2 | 82.9 (8) |
O2i—RE1—O4vi | 158.6 (5) | RE1i—O2—B2 | 147.3 (14) |
O1—RE2—O6vii | 69.0 (5) | RE1iv—O2—RE1i | 106.6 (4) |
O1—RE2—O4v | 152.1 (5) | RE3—O3—B1 | 105.4 (10) |
O1—RE2—O5vii | 85.4 (5) | RE1iii—O3—B1 | 83.9 (9) |
O1—RE2—O7 | 111.1 (5) | RE3i—O3—B1 | 105.4 (10) |
O4v—RE2—O6vii | 128.7 (6) | RE1i—O3—B1 | 154.0 (12) |
O1viii—RE2—O6vii | 55.3 (6) | RE1iii—O3—RE1i | 98.3 (5) |
O5i—RE2—O6vii | 144.8 (6) | RE1iii—O4—B1 | 83.2 (8) |
O1viii—RE2—O4v | 73.5 (4) | RE2xiv—O4—B1 | 127.1 (11) |
O1—RE2—O1viii | 120.4 (5) | RE1xv—O4—B1 | 118.4 (11) |
O1—RE2—O5i | 76.8 (4) | RE1iii—O4—RE1xv | 108.1 (6) |
O5vii—RE2—O7 | 150.4 (6) | RE2ix—O5—B1 | 90.4 (9) |
O6vii—RE2—O7 | 72.8 (5) | RE1xiv—O5—B1 | 140.1 (12) |
O4v—RE2—O7 | 95.8 (5) | RE2i—O5—B1 | 104.9 (10) |
O1viii—RE2—O7 | 72.9 (6) | RE2ix—O5—RE2i | 98.7 (6) |
O5i—RE2—O7 | 113.7 (6) | RE3—O6—B3 | 144 (2) |
O5vii—RE2—O6vii | 91.9 (6) | RE2ix—O6—B3 | 93.1 (13) |
O4v—RE2—O5vii | 73.8 (5) | RE2x—O6—B3 | 93.1 (13) |
O1viii—RE2—O5vii | 77.6 (5) | RE3i—O6—B3 | 144 (2) |
O5vii—RE2—O5i | 93.5 (5) | RE2ix—O6—RE2x | 105.7 (8) |
O4v—RE2—O5i | 86.0 (5) | RE3—O7—B2 | 133.7 (13) |
O1viii—RE2—O5i | 159.2 (5) | RE2—O7—B2 | 117.4 (8) |
O3i—RE3—B2iii | 82.7 (3) | RE2—O7—RE2i | 93.2 (6) |
O2xi—RE3—O3i | 114.0 (4) | RE3i—O7—B2 | 133.7 (13) |
O1x—RE3—O2xi | 112.8 (6) | RE2i—O7—B2 | 117.4 (8) |
O1x—RE3—O3i | 70.1 (4) | O3—B1—O4 | 107.7 (12) |
O1ix—RE3—B2iii | 109.3 (5) | O3—B1—O5 | 122.9 (13) |
O1ix—RE3—O1x | 56.4 (4) | O4—B1—O5 | 108.2 (13) |
O1ix—RE3—O2xi | 84.9 (6) | O2—B2—O7 | 99.9 (11) |
O1ix—RE3—O3i | 126.2 (4) | RE3iv—B2—O2 | 65.1 (8) |
O2iii—RE3—B2iii | 32.0 (3) | RE3xiii—B2—O2 | 65.1 (8) |
O1x—RE3—O2iii | 84.9 (6) | O2—B2—O2i | 119.6 (14) |
O2iii—RE3—O2xi | 60.6 (4) | RE3iv—B2—O7 | 143.2 (12) |
O2iii—RE3—O3i | 53.9 (4) | RE3xiii—B2—O7 | 143.2 (12) |
O1x—RE3—B2iii | 109.3 (5) | O2i—B2—O7 | 99.9 (11) |
O2xi—RE3—B2iii | 32.0 (3) | RE3iv—B2—O2i | 65.1 (8) |
O3—RE3—O6 | 97.2 (3) | RE3xiii—B2—O2i | 65.1 (8) |
O3—RE3—O7 | 84.5 (3) | O1—B3—O6 | 123.6 (17) |
O1ix—RE3—O3 | 70.1 (4) | O1—B3—O1i | 113 (3) |
O2iii—RE3—O3 | 114.0 (4) | O1i—B3—O6 | 123.6 (17) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Ho2 | b = 15.48509 (10) Å |
Mr = 685.33 | c = 8.56345 (5) Å |
Orthorhombic, Pnma | V = 948.57 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.15331 (4) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 6.35 | Rexp = 2.58 |
Rwp = 8.97 | RBragg = 4.34 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.51938 (17) | 0.08373 (8) | 0.82184 (15) | 1.49 (2) | 0.5724 (13) |
RE1 | 0.51938 (17) | 0.08373 (8) | 0.82184 (15) | 1.49 (2) | 0.4276 (13) |
Ca2 | 0.6976 (2) | 0.12756 (9) | 0.34002 (19) | 1.49 (2) | 0.7495 (10) |
RE2 | 0.6976 (2) | 0.12756 (9) | 0.34002 (19) | 1.49 (2) | 0.2505 (10) |
Ca3 | 0.32636 (19) | 0.25 | 0.53217 (16) | 1.49 (2) | 0.3563 (17) |
RE3 | 0.32636 (19) | 0.25 | 0.53217 (16) | 1.49 (2) | 0.6438 (17) |
B1 | 0.334 (3) | 0.4564 (12) | 0.452 (2) | 4.3 (4) | |
B2 | 0.715 (4) | 0.25 | 0.659 (3) | 4.3 (4) | |
B3 | 0.488 (4) | 0.25 | 0.139 (3) | 4.3 (4) | |
O1 | 0.5513 (12) | 0.1769 (5) | 0.0667 (11) | 4.52 (12) | |
O2 | 0.7520 (13) | 0.3281 (5) | 0.7240 (10) | 4.52 (12) | |
O3 | 0.3887 (14) | 0.4038 (6) | 0.5675 (12) | 4.52 (12) | |
O4 | 0.2049 (13) | 0.5150 (6) | 0.4932 (11) | 4.52 (12) | |
O5 | 0.3988 (13) | 0.4599 (6) | 0.3032 (12) | 4.52 (12) | |
O6 | 0.3717 (18) | 0.25 | 0.2646 (16) | 4.52 (12) | |
O7 | 0.6591 (19) | 0.25 | 0.5073 (15) | 4.52 (12) | |
Geometric parameters (Å, º) top
RE1—O3i | 2.378 (10) | RE3—O3i | 2.442 (9) |
RE1—O1ii | 2.556 (9) | RE3—O3 | 2.442 (9) |
RE1—O2iii | 2.383 (9) | RE3—O6 | 2.314 (14) |
RE1—O4iv | 2.571 (9) | RE3—O7 | 2.390 (14) |
RE1—O5v | 2.273 (10) | RE3—O1ix | 2.423 (9) |
RE1—O4vi | 2.421 (9) | RE3—O2iii | 2.471 (8) |
RE1—O2i | 2.310 (9) | RE3—O1x | 2.423 (9) |
RE2—O1 | 2.675 (9) | O1—B3 | 1.367 (17) |
RE2—O7 | 2.392 (8) | O2—B2 | 1.357 (14) |
RE2—O5vii | 2.326 (10) | O3—B1 | 1.34 (2) |
RE2—O6vii | 2.439 (8) | O4—B1 | 1.34 (2) |
RE2—O4v | 2.359 (9) | O5—B1 | 1.36 (2) |
RE2—O5i | 2.550 (9) | O6—B3 | 1.36 (3) |
RE3—O2viii | 2.471 (8) | O7—B2 | 1.36 (3) |
| | | |
O1ii—RE1—O4vi | 79.1 (3) | O1ix—RE3—O3i | 130.3 (3) |
O1ii—RE1—O2i | 84.2 (3) | O1x—RE3—O2iii | 83.8 (3) |
O1ii—RE1—O3i | 137.8 (3) | O2iii—RE3—O2viii | 58.6 (3) |
O2iii—RE1—O4iv | 149.0 (3) | O2iii—RE3—O3i | 57.1 (3) |
O2iii—RE1—O5v | 127.8 (3) | O1x—RE3—O2viii | 110.4 (3) |
O2iii—RE1—O4vi | 79.6 (3) | O1x—RE3—O3i | 74.7 (3) |
O2iii—RE1—O2i | 100.4 (3) | O2viii—RE3—O3i | 114.3 (3) |
O2iii—RE1—O3i | 59.1 (3) | O1ix—RE3—O7 | 141.1 (3) |
O4iv—RE1—O5v | 69.9 (3) | O2iii—RE3—O7 | 106.8 (3) |
O4iv—RE1—O4vi | 73.0 (3) | O1x—RE3—O7 | 141.1 (3) |
O2i—RE1—O4iv | 101.7 (3) | O2viii—RE3—O7 | 106.8 (3) |
O3i—RE1—O4iv | 144.7 (3) | O3—RE3—O6 | 95.6 (3) |
O4vi—RE1—O5v | 94.9 (3) | RE2—O1—B3 | 88.3 (11) |
O2i—RE1—O5v | 98.2 (3) | RE1xi—O1—B3 | 144.0 (12) |
O3i—RE1—O5v | 74.8 (3) | RE3vii—O1—B3 | 92.3 (11) |
O2i—RE1—O4vi | 163.2 (3) | RE3xii—O1—B3 | 92.3 (11) |
O3i—RE1—O4vi | 109.3 (3) | RE3iv—O2—B2 | 87.3 (11) |
O2i—RE1—O3i | 84.4 (3) | RE1iv—O2—B2 | 126.8 (13) |
O1ii—RE1—O2iii | 83.3 (3) | RE3xiii—O2—B2 | 87.3 (11) |
O1ii—RE1—O4iv | 77.5 (3) | RE1i—O2—B2 | 122.3 (13) |
O1ii—RE1—O5v | 147.1 (3) | RE1iv—O2—RE1i | 107.4 (3) |
O1—RE2—O7 | 104.6 (3) | RE3—O3—B1 | 116.6 (10) |
O1—RE2—O5vii | 87.0 (3) | RE3i—O3—B1 | 116.6 (10) |
O1—RE2—O6vii | 69.9 (4) | RE1i—O3—B1 | 137.9 (10) |
O6vii—RE2—O7 | 70.3 (4) | RE1iii—O4—B1 | 96.6 (9) |
O4v—RE2—O7 | 104.9 (3) | RE2xiv—O4—B1 | 117.1 (10) |
O5i—RE2—O7 | 113.5 (4) | RE1xv—O4—B1 | 126.4 (9) |
O5vii—RE2—O6vii | 86.7 (3) | RE1iii—O4—RE1xv | 107.0 (3) |
O1—RE2—O4v | 148.9 (3) | RE2ix—O5—B1 | 105.1 (10) |
O1—RE2—O5i | 73.5 (3) | RE1xiv—O5—B1 | 124.3 (10) |
O5vii—RE2—O7 | 148.1 (4) | RE2i—O5—B1 | 98.6 (10) |
O4v—RE2—O5i | 86.0 (3) | RE2ix—O5—RE2i | 105.9 (4) |
O5i—RE2—O6vii | 142.7 (4) | RE3—O6—B3 | 150.3 (14) |
O4v—RE2—O6vii | 130.2 (4) | RE2ix—O6—B3 | 91.3 (9) |
O4v—RE2—O5vii | 72.9 (3) | RE2x—O6—B3 | 91.3 (9) |
O5vii—RE2—O5i | 98.3 (3) | RE3i—O6—B3 | 150.3 (14) |
O1ix—RE3—O3 | 74.7 (3) | RE2ix—O6—RE2x | 102.0 (5) |
O2iii—RE3—O3 | 114.3 (3) | RE3—O7—B2 | 102.0 (14) |
O1x—RE3—O3 | 130.3 (3) | RE2—O7—B2 | 122.6 (5) |
O2viii—RE3—O3 | 57.1 (3) | RE2—O7—RE2i | 104.9 (5) |
O2iii—RE3—O6 | 150.1 (2) | RE3i—O7—B2 | 102.0 (14) |
O1x—RE3—O6 | 76.6 (4) | RE2i—O7—B2 | 122.6 (5) |
O2viii—RE3—O6 | 150.1 (2) | O3—B1—O4 | 114.7 (14) |
O3i—RE3—O6 | 95.6 (3) | O3—B1—O5 | 128.2 (16) |
O3—RE3—O3i | 154.5 (3) | O4—B1—O5 | 117.1 (14) |
O6—RE3—O7 | 76.8 (4) | O2—B2—O7 | 116.7 (11) |
O1ix—RE3—O6 | 76.6 (4) | O2—B2—O2i | 126 (2) |
O3—RE3—O7 | 80.2 (2) | O2i—B2—O7 | 116.7 (11) |
O3i—RE3—O7 | 80.2 (2) | O1—B3—O6 | 124.1 (10) |
O1ix—RE3—O2iii | 110.4 (3) | O1—B3—O1i | 111.8 (19) |
O1ix—RE3—O1x | 55.7 (3) | O1i—B3—O6 | 124.1 (10) |
O1ix—RE3—O2viii | 83.8 (3) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x−1/2, y, −z+3/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x, y, z−1; (xii) x+1/2, y, −z+1/2; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Er2 | b = 15.44654 (7) Å |
Mr = 689.99 | c = 8.54888 (4) Å |
Orthorhombic, Pnma | V = 944.29 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.15099 (3) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 6.58 | Rexp = 3.06 |
Rwp = 9.35 | RBragg = 4.89 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.51966 (16) | 0.08393 (7) | 0.82187 (14) | 1.68 (2) | 0.5682 (12) |
RE1 | 0.51966 (16) | 0.08393 (7) | 0.82187 (14) | 1.68 (2) | 0.4318 (12) |
Ca2 | 0.6979 (2) | 0.12683 (9) | 0.34039 (18) | 1.68 (2) | 0.7566 (9) |
RE2 | 0.6979 (2) | 0.12683 (9) | 0.34039 (18) | 1.68 (2) | 0.2434 (9) |
Ca3 | 0.32539 (18) | 0.25 | 0.53166 (15) | 1.68 (2) | 0.3504 (16) |
RE3 | 0.32539 (18) | 0.25 | 0.53166 (15) | 1.68 (2) | 0.6496 (16) |
B1 | 0.334 (3) | 0.4588 (12) | 0.454 (2) | 4.5 (4) | |
B2 | 0.713 (4) | 0.25 | 0.660 (3) | 4.5 (4) | |
B3 | 0.488 (4) | 0.25 | 0.135 (3) | 4.5 (4) | |
O1 | 0.5490 (12) | 0.1745 (5) | 0.0701 (10) | 4.47 (11) | |
O2 | 0.7547 (13) | 0.3266 (5) | 0.7242 (10) | 4.47 (11) | |
O3 | 0.3960 (13) | 0.4005 (5) | 0.5545 (11) | 4.47 (11) | |
O4 | 0.2037 (12) | 0.5155 (5) | 0.4890 (10) | 4.47 (11) | |
O5 | 0.3955 (12) | 0.4558 (6) | 0.3070 (12) | 4.47 (11) | |
O6 | 0.3779 (17) | 0.25 | 0.2641 (15) | 4.47 (11) | |
O7 | 0.6617 (17) | 0.25 | 0.5078 (14) | 4.47 (11) | |
Geometric parameters (Å, º) top
RE1—O3i | 2.463 (9) | RE3—O3 | 2.387 (8) |
RE1—O1ii | 2.550 (8) | RE3—O6 | 2.318 (13) |
RE1—O2iii | 2.378 (9) | RE3—O7 | 2.414 (12) |
RE1—O4iv | 2.589 (8) | RE3—O1ix | 2.454 (8) |
RE1—O5v | 2.345 (10) | RE3—O2iii | 2.452 (8) |
RE1—O4vi | 2.390 (8) | RE3—O1x | 2.454 (8) |
RE1—O2i | 2.331 (9) | RE3—O2xi | 2.452 (8) |
RE2—O1 | 2.649 (9) | O1—B3 | 1.363 (16) |
RE2—O7 | 2.395 (7) | O2—B2 | 1.338 (14) |
RE2—O5vii | 2.283 (9) | O3—B1 | 1.32 (2) |
RE2—O6vii | 2.465 (8) | O4—B1 | 1.31 (2) |
RE2—O4v | 2.362 (8) | O5—B1 | 1.33 (2) |
RE2—O1viii | 2.726 (9) | O6—B3 | 1.36 (3) |
RE2—O5i | 2.527 (9) | O7—B2 | 1.35 (3) |
RE3—O3i | 2.387 (8) | | |
| | | |
O1ii—RE1—O4vi | 78.5 (3) | O1x—RE3—O2xi | 111.4 (3) |
O1ii—RE1—O2i | 85.0 (3) | O1x—RE3—O3i | 74.7 (3) |
O1ii—RE1—O3i | 138.4 (3) | O2xi—RE3—O3i | 116.4 (3) |
O2iii—RE1—O4iv | 148.6 (3) | O1ix—RE3—O7 | 140.6 (3) |
O2iii—RE1—O5v | 128.2 (3) | O2iii—RE3—O7 | 106.1 (3) |
O2iii—RE1—O4vi | 79.8 (3) | O1x—RE3—O7 | 140.6 (3) |
O2iii—RE1—O2i | 99.8 (3) | O2xi—RE3—O7 | 106.1 (3) |
O2iii—RE1—O3i | 60.2 (3) | O3—RE3—O6 | 92.7 (2) |
O4iv—RE1—O5v | 70.2 (3) | O3—RE3—O7 | 78.2 (2) |
O4iv—RE1—O4vi | 72.8 (3) | O1ix—RE3—O3 | 74.7 (3) |
O2i—RE1—O4iv | 102.1 (3) | O2iii—RE3—O3 | 116.4 (3) |
O3i—RE1—O4iv | 145.1 (3) | O1x—RE3—O3 | 131.5 (3) |
O4vi—RE1—O5v | 94.6 (3) | O2xi—RE3—O3 | 60.3 (3) |
O2i—RE1—O5v | 98.4 (3) | O3—RE3—O3i | 153.8 (3) |
O3i—RE1—O5v | 74.9 (3) | RE2—O1—B3 | 90.7 (11) |
O2i—RE1—O4vi | 163.4 (3) | RE2—O1—RE2x | 92.9 (3) |
O3i—RE1—O4vi | 111.0 (3) | RE1xii—O1—B3 | 141.4 (12) |
O2i—RE1—O3i | 82.5 (3) | RE3vii—O1—B3 | 89.7 (11) |
O1ii—RE1—O2iii | 83.4 (3) | RE2x—O1—B3 | 79.8 (11) |
O1ii—RE1—O4iv | 76.4 (3) | RE3viii—O1—B3 | 89.7 (11) |
O1ii—RE1—O5v | 146.4 (3) | RE3iv—O2—B2 | 88.2 (11) |
O1—RE2—O7 | 104.9 (3) | RE1iv—O2—B2 | 128.6 (13) |
O1—RE2—O5vii | 85.6 (3) | RE3xiii—O2—B2 | 88.2 (11) |
O1—RE2—O6vii | 71.3 (3) | RE1i—O2—B2 | 120.7 (13) |
O5vii—RE2—O7 | 147.2 (4) | RE1iv—O2—RE1i | 106.8 (3) |
O6vii—RE2—O7 | 70.1 (3) | RE3—O3—B1 | 122.7 (10) |
O4v—RE2—O7 | 104.0 (3) | RE3i—O3—B1 | 122.7 (10) |
O1viii—RE2—O7 | 73.6 (3) | RE1i—O3—B1 | 131.1 (9) |
O1—RE2—O4v | 149.4 (3) | RE1iii—O4—B1 | 96.2 (9) |
O1—RE2—O1viii | 122.7 (3) | RE2xiv—O4—B1 | 114.5 (10) |
O1—RE2—O5i | 72.4 (3) | RE1xv—O4—B1 | 129.3 (9) |
O5vii—RE2—O5i | 100.7 (3) | RE1iii—O4—RE1xv | 107.2 (3) |
O4v—RE2—O6vii | 129.1 (3) | RE2ix—O5—B1 | 109.6 (10) |
O1viii—RE2—O6vii | 54.0 (3) | RE1xiv—O5—B1 | 120.0 (10) |
O5i—RE2—O6vii | 142.7 (4) | RE2i—O5—B1 | 101.2 (10) |
O1viii—RE2—O4v | 75.5 (3) | RE2ix—O5—RE2i | 108.0 (4) |
O4v—RE2—O5i | 87.5 (3) | RE3—O6—B3 | 153.8 (14) |
O1viii—RE2—O5i | 163.0 (3) | RE2ix—O6—B3 | 90.5 (9) |
O5vii—RE2—O6vii | 84.7 (3) | RE2x—O6—B3 | 90.5 (9) |
O4v—RE2—O5vii | 75.5 (3) | RE3i—O6—B3 | 153.8 (14) |
O1viii—RE2—O5vii | 74.7 (3) | RE2ix—O6—RE2x | 101.1 (4) |
O5i—RE2—O7 | 112.1 (4) | RE3—O7—B2 | 100.9 (14) |
O2xi—RE3—O6 | 150.86 (19) | RE2—O7—B2 | 123.1 (5) |
O3i—RE3—O6 | 92.7 (2) | RE2—O7—RE2i | 105.2 (5) |
O1x—RE3—O6 | 77.3 (3) | RE3i—O7—B2 | 100.9 (14) |
O6—RE3—O7 | 75.8 (4) | RE2i—O7—B2 | 123.1 (5) |
O1ix—RE3—O6 | 77.3 (3) | O3—B1—O4 | 123.0 (15) |
O2iii—RE3—O6 | 150.86 (19) | O3—B1—O5 | 118.6 (16) |
O3i—RE3—O7 | 78.2 (2) | O4—B1—O5 | 118.2 (15) |
O1ix—RE3—O2iii | 111.4 (3) | O2—B2—O7 | 117.1 (11) |
O1ix—RE3—O1x | 56.7 (3) | O2—B2—O2i | 124 (2) |
O1ix—RE3—O2xi | 84.6 (3) | O2i—B2—O7 | 117.1 (11) |
O1ix—RE3—O3i | 131.5 (3) | O1—B3—O6 | 121.1 (10) |
O1x—RE3—O2iii | 84.6 (3) | O1—B3—O1i | 118 (2) |
O2iii—RE3—O2xi | 57.7 (3) | O1i—B3—O6 | 121.1 (10) |
O2iii—RE3—O3i | 60.3 (3) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |
Crystal data top
B4Ca3O12Y2 | b = 15.47341 (4) Å |
Mr = 533.28 | c = 8.559253 (19) Å |
Orthorhombic, Pnma | V = 947.51 (1) Å3 |
Hall symbol: -P 2ac 2n | Z = 4 |
a = 7.154177 (16) Å | T = 295 K |
Data collection top
ID22 diffractometer, transmission geometry | 2θmin = 0.502°, 2θmax = 40.00°, 2θstep = 0.002° |
Refinement top
Rp = 8.89 | Rexp = 3.58 |
Rwp = 12.81 | RBragg = 8.80 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | Occ. (<1) |
Ca1 | 0.52125 (19) | 0.08358 (9) | 0.82098 (17) | 1.37 (2) | 0.570 (3) |
RE1 | 0.52125 (19) | 0.08358 (9) | 0.82098 (17) | 1.37 (2) | 0.430 (3) |
Ca2 | 0.6996 (2) | 0.12647 (10) | 0.3425 (2) | 1.37 (2) | 0.772 (2) |
RE2 | 0.6996 (2) | 0.12647 (10) | 0.3425 (2) | 1.37 (2) | 0.228 (2) |
Ca3 | 0.3255 (2) | 0.25 | 0.53121 (19) | 1.37 (2) | 0.317 (3) |
RE3 | 0.3255 (2) | 0.25 | 0.53121 (19) | 1.37 (2) | 0.683 (3) |
B1 | 0.325 (2) | 0.4561 (11) | 0.452 (2) | 6.1 (4) | |
B2 | 0.670 (3) | 0.25 | 0.661 (3) | 6.1 (4) | |
B3 | 0.488 (4) | 0.25 | 0.139 (3) | 6.1 (4) | |
O1 | 0.5533 (10) | 0.1758 (5) | 0.0683 (9) | 4.72 (9) | |
O2 | 0.7612 (11) | 0.3221 (5) | 0.7213 (9) | 4.72 (9) | |
O3 | 0.3961 (11) | 0.4015 (5) | 0.5568 (10) | 4.72 (9) | |
O4 | 0.2037 (10) | 0.5176 (5) | 0.4864 (9) | 4.72 (9) | |
O5 | 0.4017 (10) | 0.4530 (5) | 0.3082 (10) | 4.72 (9) | |
O6 | 0.3746 (14) | 0.25 | 0.2665 (13) | 4.72 (9) | |
O7 | 0.6539 (14) | 0.25 | 0.5034 (13) | 4.72 (9) | |
Geometric parameters (Å, º) top
RE1—O3i | 2.443 (9) | RE3—O3 | 2.408 (8) |
RE1—O1ii | 2.563 (8) | RE3—O6 | 2.293 (11) |
RE1—O2iii | 2.392 (8) | RE3—O7 | 2.362 (10) |
RE1—O4iv | 2.622 (8) | RE3—O1ix | 2.416 (7) |
RE1—O5v | 2.368 (8) | RE3—O2iii | 2.438 (8) |
RE1—O4vi | 2.374 (8) | RE3—O1x | 2.416 (7) |
RE1—O2i | 2.409 (8) | RE3—O2xi | 2.438 (8) |
RE2—O1 | 2.681 (8) | O1—B3 | 1.379 (17) |
RE2—O7 | 2.379 (7) | O2—B2 | 1.392 (16) |
RE2—O5vii | 2.295 (8) | O3—B1 | 1.333 (19) |
RE2—O6vii | 2.468 (7) | O4—B1 | 1.321 (18) |
RE2—O4v | 2.337 (8) | O5—B1 | 1.349 (19) |
RE2—O1viii | 2.751 (7) | O6—B3 | 1.36 (3) |
RE2—O5i | 2.478 (7) | O7—B2 | 1.35 (3) |
RE3—O3i | 2.408 (8) | | |
| | | |
O1ii—RE1—O4vi | 78.9 (3) | O1x—RE3—O2xi | 111.8 (3) |
O1ii—RE1—O2i | 83.8 (3) | O1x—RE3—O3i | 74.8 (3) |
O1ii—RE1—O3i | 138.1 (3) | O2xi—RE3—O3i | 114.0 (3) |
O2iii—RE1—O4iv | 147.9 (3) | O1ix—RE3—O7 | 140.0 (3) |
O2iii—RE1—O5v | 129.1 (3) | O2iii—RE3—O7 | 106.0 (3) |
O2iii—RE1—O4vi | 79.9 (3) | O1x—RE3—O7 | 140.0 (3) |
O2iii—RE1—O2i | 97.5 (3) | O2xi—RE3—O7 | 106.0 (3) |
O2iii—RE1—O3i | 61.1 (3) | O3—RE3—O6 | 93.3 (2) |
O4iv—RE1—O5v | 70.6 (3) | O3—RE3—O7 | 78.49 (19) |
O4iv—RE1—O4vi | 72.9 (2) | O1ix—RE3—O3 | 74.8 (3) |
O2i—RE1—O4iv | 103.3 (2) | O2iii—RE3—O3 | 114.0 (3) |
O3i—RE1—O4iv | 145.2 (3) | O1x—RE3—O3 | 131.6 (3) |
O4vi—RE1—O5v | 94.0 (3) | O2xi—RE3—O3 | 61.0 (3) |
O2i—RE1—O5v | 100.7 (3) | O3—RE3—O3i | 153.6 (3) |
O3i—RE1—O5v | 74.6 (3) | RE2—O1—B3 | 89.2 (11) |
O2i—RE1—O4vi | 162.7 (3) | RE2—O1—RE2x | 92.1 (2) |
O3i—RE1—O4vi | 110.1 (3) | RE1xii—O1—B3 | 142.7 (12) |
O2i—RE1—O3i | 82.9 (3) | RE3vii—O1—B3 | 91.8 (11) |
O1ii—RE1—O2iii | 81.7 (3) | RE2x—O1—B3 | 78.3 (11) |
O1ii—RE1—O4iv | 76.6 (2) | RE3viii—O1—B3 | 91.8 (11) |
O1ii—RE1—O5v | 147.1 (3) | RE3iv—O2—B2 | 92.5 (10) |
O1—RE2—O7 | 103.0 (3) | RE1iv—O2—B2 | 142.9 (11) |
O1—RE2—O5vii | 84.6 (3) | RE3xiii—O2—B2 | 92.5 (10) |
O1—RE2—O6vii | 69.3 (3) | RE1i—O2—B2 | 106.4 (9) |
O5vii—RE2—O7 | 147.4 (3) | RE1iv—O2—RE1i | 103.8 (3) |
O6vii—RE2—O7 | 70.5 (3) | RE3—O3—B1 | 118.4 (9) |
O4v—RE2—O7 | 104.9 (3) | RE3i—O3—B1 | 118.4 (9) |
O1viii—RE2—O7 | 75.1 (3) | RE1i—O3—B1 | 134.7 (9) |
O1—RE2—O4v | 150.4 (3) | RE1iii—O4—B1 | 92.1 (8) |
O1—RE2—O1viii | 121.5 (2) | RE2xiv—O4—B1 | 117.7 (8) |
O1—RE2—O5i | 72.7 (3) | RE1xv—O4—B1 | 128.5 (9) |
O5vii—RE2—O5i | 102.1 (3) | RE1iii—O4—RE1xv | 107.1 (3) |
O4v—RE2—O6vii | 130.2 (3) | RE2ix—O5—B1 | 106.0 (8) |
O1viii—RE2—O6vii | 54.8 (3) | RE1xiv—O5—B1 | 119.4 (9) |
O5i—RE2—O6vii | 140.9 (3) | RE2i—O5—B1 | 105.0 (8) |
O1viii—RE2—O4v | 75.8 (2) | RE2ix—O5—RE2i | 110.0 (3) |
O4v—RE2—O5i | 88.4 (3) | RE3—O6—B3 | 152.2 (13) |
O1viii—RE2—O5i | 164.1 (3) | RE2ix—O6—B3 | 90.0 (8) |
O5vii—RE2—O6vii | 83.3 (3) | RE2x—O6—B3 | 90.0 (8) |
O4v—RE2—O5vii | 77.3 (3) | RE3i—O6—B3 | 152.2 (13) |
O1viii—RE2—O5vii | 74.1 (3) | RE2ix—O6—RE2x | 101.5 (4) |
O5i—RE2—O7 | 110.4 (3) | RE3—O7—B2 | 89.1 (10) |
O2xi—RE3—O6 | 152.57 (18) | RE2—O7—B2 | 124.4 (3) |
O3i—RE3—O6 | 93.3 (2) | RE2—O7—RE2i | 107.0 (4) |
O1x—RE3—O6 | 77.0 (3) | RE3i—O7—B2 | 89.1 (10) |
O6—RE3—O7 | 75.4 (4) | RE2i—O7—B2 | 124.4 (3) |
O1ix—RE3—O6 | 77.0 (3) | O3—B1—O4 | 123.9 (14) |
O2iii—RE3—O6 | 152.57 (18) | O3—B1—O5 | 115.9 (12) |
O3i—RE3—O7 | 78.49 (19) | O4—B1—O5 | 119.8 (13) |
O1ix—RE3—O2iii | 111.8 (3) | O2—B2—O7 | 114.2 (12) |
O1ix—RE3—O1x | 56.8 (3) | O2—B2—O2i | 106.6 (16) |
O1ix—RE3—O2xi | 86.4 (3) | O2i—B2—O7 | 114.2 (12) |
O1ix—RE3—O3i | 131.6 (3) | O1—B3—O6 | 123.7 (10) |
O1x—RE3—O2iii | 86.4 (3) | O1—B3—O1i | 112.7 (19) |
O2iii—RE3—O2xi | 54.5 (3) | O1i—B3—O6 | 123.7 (10) |
O2iii—RE3—O3i | 61.0 (3) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x−1/2, −y+1/2, −z+3/2; (iv) x+1/2, −y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+1; (vi) −x+1/2, y−1/2, z+1/2; (vii) x+1/2, −y+1/2, −z+1/2; (viii) x+1/2, y, −z+1/2; (ix) x−1/2, −y+1/2, −z+1/2; (x) x−1/2, y, −z+1/2; (xi) x−1/2, y, −z+3/2; (xii) x, y, z−1; (xiii) x+1/2, y, −z+3/2; (xiv) −x+1, y+1/2, −z+1; (xv) −x+1/2, y+1/2, z−1/2. |