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The classical external-standard method derived from the work of O'Connor & Raven [Powder Diffr. (1988), 3, 2-6] was used to examine the hydration of the major phase, alite, of ordinary Portland cements at different temperatures and different water/alite ratios. In order to estimate the accuracy of the method, heat-flow curves were calculated from the alite dissolution curves obtained from X-ray diffraction in situ experiments. The heat-flow curves calculated in this way were compared with heat-flow curves recorded using a calorimeter. It is shown that the calculated curves agree well with the curves obtained from heat-flow experiments.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889811025933/cg5188sup1.cif
Contains datablocks global, Synthesized_Alite

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889811025933/cg5188SynthesizedAlitesup2.rtv
Contains datablock Synthesized_Alite

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889811025933/cg5188sup3.cif
Contains datablocks global, Alite_Hydration_11h, Portlandite

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889811025933/cg5188AliteHydration11hsup4.rtv
Contains datablock Alite_Hydration_11h

Computing details top

For both compounds, data collection: XRD Commander ((Bruker); cell refinement: TOPAS V.4.2 (Bruker); data reduction: -; program(s) used to solve structure: -; program(s) used to refine structure: -; molecular graphics: -; software used to prepare material for publication: -.

'Tricalcium Silicate Oxide' top
Crystal data top
Ca3O5SiZ = 36
Monoclinic, CmCu Kα1 radiation, λ = 1.5406 Å
a = 33.085 ÅT = 298 K
b = 7.037 Åwhite
c = 18.521 Åflat_sheet, 22 × 22 mm
β = 94.159°Specimen preparation: Prepared at 298 K and 101.325 kPa
V = 4300.7 Å3
Data collection top
D8 Bruker
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tube, KFL CU 2K SiemensScan method: step
None monochromator2θmin = 7.0°, 2θmax = 70.018°, 2θstep = 0.022°
Specimen mounting: sample holder (PMMA)
Refinement top
Least-squares matrix: fullExcluded region(s): none
Rp = 0.043Profile function: fundamental parameter type peaks in a non linear least-squares refinement
Rwp = 0.083
Rexp = 0.037Background function: Chebychev polynomial 6th order
2822 data pointsPreferred orientation correction: none
Special details top

Experimental. powder sample

Refinement. Hatrurite structure from "De La Torre, A. G., Bruque, S., Campo, S. & Aranda, M. (2002). The superstructure of C3S from synchroton and neutron powder diffraction and its role in quantitative phase analysis. Cement and Concrete Research, 32, 1347-1356." was used for refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.0024 (1)00.0104 (19)0.012 (1)
Ca20.6595 (10)00.1605 (19)0.012 (1)
Ca30.3113 (9)00.3342 (19)0.012 (1)
Ca40.0119 (12)00.4939 (19)0.012 (1)
Ca50.6531 (11)00.6651 (18)0.012 (1)
Ca60.3188 (11)00.8407 (19)0.012 (1)
Ca70.5881 (11)00.075 (2)0.012 (1)
Ca80.2592 (11)00.1012 (19)0.012 (1)
Ca90.0815 (11)00.2619 (19)0.012 (1)
Ca100.5848 (9)00.4262 (18)0.012 (1)
Ca110.2494 (11)00.6061 (19)0.012 (1)
Ca120.0817 (11)00.765 (2)0.012 (1)
Ca130.7322 (11)00.0925 (19)0.012 (1)
Ca140.4019 (11)00.078 (2)0.012 (1)
Ca150.0646 (10)00.2418 (19)0.012 (1)
Ca160.7236 (10)00.402 (2)0.012 (1)
Ca170.3895 (11)00.573 (2)0.012 (1)
Ca180.0617 (11)00.7363 (19)0.012 (1)
Ca190.0835 (10)0.275 (3)0.085 (2)0.0104 (8)0.5
Ca200.0833 (10)0.275 (3)0.085 (2)0.0104 (8)0.5
Ca210.5804 (12)0.277 (3)0.084 (2)0.0104 (8)0.5
Ca220.5849 (11)0.281 (2)0.0917 (18)0.0104 (8)0.5
Ca230.2398 (11)0.250 (3)0.2580 (18)0.0104 (8)0.5
Ca240.2413 (11)0.257 (3)0.2577 (18)0.0104 (8)0.5
Ca250.0969 (11)0.265 (4)0.4132 (18)0.0104 (8)0.5
Ca260.0938 (11)0.293 (3)0.4099 (18)0.0104 (8)0.5
Ca270.5759 (13)0.250 (4)0.597 (2)0.0104 (8)0.5
Ca280.5651 (11)0.223 (4)0.572 (2)0.0104 (8)0.5
Ca290.2436 (11)0.250 (4)0.752 (3)0.0104 (8)0.5
Ca300.2444 (10)0.241 (3)0.762 (2)0.0104 (8)0.5
Ca310.0023 (14)0.218 (5)0.847 (3)0.0104 (8)0.5
Ca320.0004 (14)0.232 (5)0.842 (3)0.0104 (8)0.5
Ca330.6675 (10)0.232 (3)0.015 (3)0.0104 (8)0.5
Ca340.6662 (10)0.241 (3)0.020 (3)0.0104 (8)0.5
Ca350.3345 (12)0.235 (4)0.172 (2)0.0104 (8)0.5
Ca360.3388 (10)0.222 (3)0.1825 (18)0.0104 (8)0.5
Ca370.0049 (10)0.235 (3)0.346 (2)0.0104 (8)0.5
Ca380.0051 (11)0.238 (3)0.3444 (19)0.0104 (8)0.5
Ca390.6608 (10)0.229 (3)0.5199 (18)0.0104 (8)0.5
Ca400.6570 (10)0.218 (2)0.5225 (17)0.0104 (8)0.5
Ca410.3312 (10)0.240 (4)0.681 (2)0.0104 (8)0.5
Ca420.3310 (10)0.236 (4)0.677 (3)0.0104 (8)0.5
Ca430.8260 (13)0.270 (4)0.012 (2)0.0104 (8)0.5
Ca440.8268 (10)0.264 (3)0.0093 (19)0.0104 (8)0.5
Ca450.4904 (10)0.260 (4)0.1593 (19)0.0104 (8)0.5
Ca460.4906 (10)0.257 (4)0.160 (2)0.0104 (8)0.5
Ca470.1502 (10)0.254 (4)0.3293 (19)0.0104 (8)0.5
Ca480.1509 (9)0.254 (3)0.3288 (19)0.0104 (8)0.5
Ca490.8127 (11)0.260 (3)0.493 (2)0.0104 (8)0.5
Ca500.8139 (10)0.261 (3)0.500 (2)0.0104 (8)0.5
Ca510.4826 (13)0.277 (5)0.6571 (19)0.0104 (8)0.5
Ca520.4821 (12)0.266 (4)0.6563 (19)0.0104 (8)0.5
Ca530.1558 (11)0.272 (3)0.8212 (19)0.0104 (8)0.5
Ca540.1554 (10)0.271 (3)0.8206 (18)0.0104 (8)0.5
Si10.0816 (11)00.4254 (19)0.004 (1)
Si20.2329 (11)00.0728 (19)0.004 (1)
Si30.4211 (11)00.747 (2)0.004 (1)
Si40.5603 (11)00.758 (2)0.004 (1)
Si50.0976 (10)00.0775 (17)0.004 (1)
Si60.8946 (10)00.5743 (18)0.004 (1)
Si70.0917 (10)00.0895 (19)0.004 (1)
Si80.1615 (10)00.1677 (18)0.004 (1)
Si90.1588 (11)00.6621 (18)0.004 (1)
Si100.2243 (9)00.4237 (17)0.004 (1)
Si110.4176 (4)00.2554 (8)0.004 (1)
Si120.5020 (10)00.0003 (19)0.004 (1)
Si130.4845 (10)00.4913 (18)0.004 (1)
Si140.5669 (9)00.2431 (17)0.004 (1)
Si150.7532 (10)00.0911 (19)0.004 (1)
Si160.7506 (10)00.5842 (19)0.004 (1)
Si170.8250 (11)00.3337 (19)0.004 (1)
Si180.8243 (11)00.8424 (19)0.004 (1)
O10.9921 (13)00.252 (2)0.031 (2)
O20.0342 (11)00.122 (2)0.031 (2)
O30.0309 (15)00.602 (4)0.031 (2)
O40.0101 (14)00.749 (2)0.031 (2)
O50.3664 (11)00.067 (3)0.031 (2)
O60.3313 (13)00.0836 (19)0.031 (2)
O70.2830 (12)00.2215 (19)0.031 (2)
O80.3525 (13)00.444 (2)0.031 (2)
O90.325 (2)00.593 (3)0.031 (2)
O100.2857 (13)00.723 (2)0.031 (2)
O110.6617 (13)00.084 (2)0.031 (2)
O120.6170 (9)00.0406 (19)0.031 (2)
O130.6976 (10)00.298 (2)0.031 (2)
O140.6537 (10)00.4255 (19)0.031 (2)
O150.6147 (11)00.550 (2)0.031 (2)
O160.7014 (13)00.770 (2)0.031 (2)
O170.9399 (13)00.387 (2)0.031 (2)
O180.9564 (13)00.903 (3)0.031 (2)
O190.1052 (13)00.3522 (19)0.016 (1)
O200.0327 (11)00.410 (2)0.016 (1)
O210.0937 (11)0.187 (2)0.4744 (19)0.016 (1)
O220.2096 (12)00.001 (2)0.016 (1)
O230.2806 (11)00.053 (2)0.016 (1)
O240.2187 (11)0.1794 (17)0.8763 (19)0.016 (1)
O250.4415 (13)00.671 (2)0.016 (1)
O260.3718 (10)00.7387 (15)0.016 (1)
O270.4338 (10)0.190 (2)0.793 (2)0.016 (1)
O280.5376 (13)00.832 (2)0.016 (1)
O290.6091 (11)00.770 (3)0.016 (1)
O300.5460 (10)0.1822 (17)0.709 (2)0.016 (1)
O310.8757 (12)00.1492 (19)0.016 (1)
O320.0504 (11)00.107 (3)0.016 (1)
O330.8933 (11)0.190 (2)0.0297 (17)0.016 (1)
O340.8717 (14)00.650 (2)0.016 (1)
O350.0569 (10)00.592 (2)0.016 (1)
O360.8832 (10)0.1887 (17)0.5270 (17)0.016 (1)
O370.1130 (12)00.8333 (19)0.016 (1)
O380.0435 (10)00.898 (3)0.016 (1)
O390.1071 (11)0.1873 (16)0.0459 (19)0.016 (1)
O400.1382 (12)0.030 (5)0.088 (2)0.016 (1)0.5
O410.1298 (11)0.875 (4)0.213 (2)0.016 (1)0.5
O420.2003 (10)0.864 (4)0.154 (2)0.016 (1)0.5
O430.1732 (12)0.191 (2)0.2111 (18)0.016 (1)0.5
O440.1803 (13)00.5844 (19)0.016 (1)0.41 (3)
O450.1104 (11)00.648 (3)0.016 (1)0.41 (3)
O460.1762 (12)0.185 (2)0.7047 (19)0.016 (1)0.41 (3)
O470.1953 (13)00.726 (3)0.016 (1)0.59 (3)
O480.1776 (12)00.583 (2)0.016 (1)0.59 (3)
O490.1303 (12)0.188 (2)0.669 (3)0.016 (1)0.59 (3)
O500.2397 (11)00.3421 (18)0.016 (1)0.41 (3)
O510.2642 (13)00.481 (2)0.016 (1)0.41 (3)
O520.1998 (11)0.1918 (16)0.430 (2)0.016 (1)0.41 (3)
O530.1873 (14)00.480 (3)0.016 (1)0.59 (3)
O540.2644 (12)00.478 (3)0.016 (1)0.59 (3)
O550.2186 (10)0.1926 (19)0.3763 (18)0.016 (1)0.59 (3)
O560.4467 (10)00.3284 (15)0.016 (1)
O570.3699 (7)00.268 (2)0.016 (1)
O580.4281 (9)0.179 (2)0.2041 (15)0.016 (1)
O590.4706 (11)00.070 (2)0.016 (1)
O600.4794 (15)00.076 (2)0.016 (1)
O610.5329 (9)0.1844 (17)0.003 (2)0.016 (1)
O620.5126 (10)00.4235 (18)0.016 (1)
O630.4357 (10)00.471 (2)0.016 (1)
O640.4939 (11)0.1927 (19)0.5364 (17)0.016 (1)
O650.5623 (14)00.1528 (18)0.016 (5)0.41 (5)
O660.6162 (10)00.260 (2)0.016 (5)0.41 (5)
O670.5482 (12)0.193 (2)0.272 (2)0.016 (5)0.41 (5)
O680.6030 (10)00.3053 (19)0.016 (5)0.59 (5)
O690.5860 (12)00.1658 (18)0.016 (5)0.59 (5)
O700.5393 (9)0.1866 (17)0.2549 (19)0.016 (5)0.59 (5)
O710.7352 (11)00.1707 (19)0.016 (5)
O720.7138 (10)00.032 (2)0.016 (5)
O730.7815 (10)0.187 (2)0.0832 (19)0.016 (5)
O740.7689 (11)00.507 (2)0.016 (5)
O750.7020 (10)00.579 (2)0.016 (5)
O760.7646 (10)0.1836 (17)0.6330 (19)0.016 (5)
O770.8031 (11)0.092 (5)0.262 (2)0.016 (5)0.5
O780.7934 (13)0.844 (5)0.363 (3)0.016 (5)0.5
O790.8635 (12)0.867 (4)0.315 (2)0.016 (5)0.5
O800.8444 (12)0.123 (4)0.400 (2)0.016 (5)0.5
O810.8038 (11)00.0796 (19)0.016 (5)
O820.8726 (11)00.859 (2)0.016 (5)
O830.8095 (12)0.191 (2)0.7989 (19)0.016 (5)
 
(Alite_Hydration_11h) 'Tricalcium Silicate Oxide' top
Crystal data top
Ca3O5SiZ = 36
Monoclinic, CmCu Kα1 radiation, λ = 1.5406 Å
a = 33.085 ÅT = 310 K
b = 7.037 Åwhite
c = 18.521 Åflat_sheet, 22 × 22 mm
β = 94.160°Specimen preparation: Prepared at 310 K and 101.325 kPa
V = 4300.6 Å3
Data collection top
D8 Bruker
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tube, KFL CU 2K SiemensScan method: step
None monochromator2θmin = 7.0°, 2θmax = 39.996°, 2θstep = 0.024°
Specimen mounting: temperated sample holder (PMMA) with Kapton film cover
Refinement top
Least-squares matrix: fullExcluded region(s): none
Rp = 0.043Profile function: fundamental parameter type peaks in a non linear least-squares refinement
Rwp = 0.061
Rexp = 0.033Background function: combination of Chebychev polynomial 0th order and fundamental parameter type peaks phase
1396 data pointsPreferred orientation correction: spherical harmonics function
Special details top

Experimental. In-situ experiment with special cooling/heating device for temperature constancy.

Refinement. Hatrurite structure from "De La Torre, A. G., Bruque, S., Campo, S. & Aranda, M. (2002). The superstructure of C3S from synchroton and neutron powder diffraction and its role in quantitative phase analysis. Cement and Concrete Research, 32, 1347-1356." was used for refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.0024 (1)00.0104 (19)0.012 (1)
Ca20.6595 (10)00.1605 (19)0.012 (1)
Ca30.3113 (9)00.3342 (19)0.012 (1)
Ca40.0119 (12)00.4939 (19)0.012 (1)
Ca50.6531 (11)00.6651 (18)0.012 (1)
Ca60.3188 (11)00.8407 (19)0.012 (1)
Ca70.5881 (11)00.075 (2)0.012 (1)
Ca80.2592 (11)00.1012 (19)0.012 (1)
Ca90.0815 (11)00.2619 (19)0.012 (1)
Ca100.5848 (9)00.4262 (18)0.012 (1)
Ca110.2494 (11)00.6061 (19)0.012 (1)
Ca120.0817 (11)00.765 (2)0.012 (1)
Ca130.7322 (11)00.0925 (19)0.012 (1)
Ca140.4019 (11)00.078 (2)0.012 (1)
Ca150.0646 (10)00.2418 (19)0.012 (1)
Ca160.7236 (10)00.402 (2)0.012 (1)
Ca170.3895 (11)00.573 (2)0.012 (1)
Ca180.0617 (11)00.7363 (19)0.012 (1)
Ca190.0835 (10)0.275 (3)0.085 (2)0.0104 (8)0.5
Ca200.0833 (10)0.275 (3)0.085 (2)0.0104 (8)0.5
Ca210.5804 (12)0.277 (3)0.084 (2)0.0104 (8)0.5
Ca220.5849 (11)0.281 (2)0.0917 (18)0.0104 (8)0.5
Ca230.2398 (11)0.250 (3)0.2580 (18)0.0104 (8)0.5
Ca240.2413 (11)0.257 (3)0.2577 (18)0.0104 (8)0.5
Ca250.0969 (11)0.265 (4)0.4132 (18)0.0104 (8)0.5
Ca260.0938 (11)0.293 (3)0.4099 (18)0.0104 (8)0.5
Ca270.5759 (13)0.250 (4)0.597 (2)0.0104 (8)0.5
Ca280.5651 (11)0.223 (4)0.572 (2)0.0104 (8)0.5
Ca290.2436 (11)0.250 (4)0.752 (3)0.0104 (8)0.5
Ca300.2444 (10)0.241 (3)0.762 (2)0.0104 (8)0.5
Ca310.0023 (14)0.218 (5)0.847 (3)0.0104 (8)0.5
Ca320.0004 (14)0.232 (5)0.842 (3)0.0104 (8)0.5
Ca330.6675 (10)0.232 (3)0.015 (3)0.0104 (8)0.5
Ca340.6662 (10)0.241 (3)0.020 (3)0.0104 (8)0.5
Ca350.3345 (12)0.235 (4)0.172 (2)0.0104 (8)0.5
Ca360.3388 (10)0.222 (3)0.1825 (18)0.0104 (8)0.5
Ca370.0049 (10)0.235 (3)0.346 (2)0.0104 (8)0.5
Ca380.0051 (11)0.238 (3)0.3444 (19)0.0104 (8)0.5
Ca390.6608 (10)0.229 (3)0.5199 (18)0.0104 (8)0.5
Ca400.6570 (10)0.218 (2)0.5225 (17)0.0104 (8)0.5
Ca410.3312 (10)0.240 (4)0.681 (2)0.0104 (8)0.5
Ca420.3310 (10)0.236 (4)0.677 (3)0.0104 (8)0.5
Ca430.8260 (13)0.270 (4)0.012 (2)0.0104 (8)0.5
Ca440.8268 (10)0.264 (3)0.0093 (19)0.0104 (8)0.5
Ca450.4904 (10)0.260 (4)0.1593 (19)0.0104 (8)0.5
Ca460.4906 (10)0.257 (4)0.160 (2)0.0104 (8)0.5
Ca470.1502 (10)0.254 (4)0.3293 (19)0.0104 (8)0.5
Ca480.1509 (9)0.254 (3)0.3288 (19)0.0104 (8)0.5
Ca490.8127 (11)0.260 (3)0.493 (2)0.0104 (8)0.5
Ca500.8139 (10)0.261 (3)0.500 (2)0.0104 (8)0.5
Ca510.4826 (13)0.277 (5)0.6571 (19)0.0104 (8)0.5
Ca520.4821 (12)0.266 (4)0.6563 (19)0.0104 (8)0.5
Ca530.1558 (11)0.272 (3)0.8212 (19)0.0104 (8)0.5
Ca540.1554 (10)0.271 (3)0.8206 (18)0.0104 (8)0.5
Si10.0816 (11)00.4254 (19)0.004 (1)
Si20.2329 (11)00.0728 (19)0.004 (1)
Si30.4211 (11)00.747 (2)0.004 (1)
Si40.5603 (11)00.758 (2)0.004 (1)
Si50.0976 (10)00.0775 (17)0.004 (1)
Si60.8946 (10)00.5743 (18)0.004 (1)
Si70.0917 (10)00.0895 (19)0.004 (1)
Si80.1615 (10)00.1677 (18)0.004 (1)
Si90.1588 (11)00.6621 (18)0.004 (1)
Si100.2243 (9)00.4237 (17)0.004 (1)
Si110.4176 (4)00.2554 (8)0.004 (1)
Si120.5020 (10)00.0003 (19)0.004 (1)
Si130.4845 (10)00.4913 (18)0.004 (1)
Si140.5669 (9)00.2431 (17)0.004 (1)
Si150.7532 (10)00.0911 (19)0.004 (1)
Si160.7506 (10)00.5842 (19)0.004 (1)
Si170.8250 (11)00.3337 (19)0.004 (1)
Si180.8243 (11)00.8424 (19)0.004 (1)
O10.9921 (13)00.252 (2)0.031 (2)
O20.0342 (11)00.122 (2)0.031 (2)
O30.0309 (15)00.602 (4)0.031 (2)
O40.0101 (14)00.749 (2)0.031 (2)
O50.3664 (11)00.067 (3)0.031 (2)
O60.3313 (13)00.0836 (19)0.031 (2)
O70.2830 (12)00.2215 (19)0.031 (2)
O80.3525 (13)00.444 (2)0.031 (2)
O90.325 (2)00.593 (3)0.031 (2)
O100.2857 (13)00.723 (2)0.031 (2)
O110.6617 (13)00.084 (2)0.031 (2)
O120.6170 (9)00.0406 (19)0.031 (2)
O130.6976 (10)00.298 (2)0.031 (2)
O140.6537 (10)00.4255 (19)0.031 (2)
O150.6147 (11)00.550 (2)0.031 (2)
O160.7014 (13)00.770 (2)0.031 (2)
O170.9399 (13)00.387 (2)0.031 (2)
O180.9564 (13)00.903 (3)0.031 (2)
O190.1052 (13)00.3522 (19)0.016 (1)
O200.0327 (11)00.410 (2)0.016 (1)
O210.0937 (11)0.187 (2)0.4744 (19)0.016 (1)
O220.2096 (12)00.001 (2)0.016 (1)
O230.2806 (11)00.053 (2)0.016 (1)
O240.2187 (11)0.1794 (17)0.8763 (19)0.016 (1)
O250.4415 (13)00.671 (2)0.016 (1)
O260.3718 (10)00.7387 (15)0.016 (1)
O270.4338 (10)0.190 (2)0.793 (2)0.016 (1)
O280.5376 (13)00.832 (2)0.016 (1)
O290.6091 (11)00.770 (3)0.016 (1)
O300.5460 (10)0.1822 (17)0.709 (2)0.016 (1)
O310.8757 (12)00.1492 (19)0.016 (1)
O320.0504 (11)00.107 (3)0.016 (1)
O330.8933 (11)0.190 (2)0.0297 (17)0.016 (1)
O340.8717 (14)00.650 (2)0.016 (1)
O350.0569 (10)00.592 (2)0.016 (1)
O360.8832 (10)0.1887 (17)0.5270 (17)0.016 (1)
O370.1130 (12)00.8333 (19)0.016 (1)
O380.0435 (10)00.898 (3)0.016 (1)
O390.1071 (11)0.1873 (16)0.0459 (19)0.016 (1)
O400.1382 (12)0.030 (5)0.088 (2)0.016 (1)0.5
O410.1298 (11)0.875 (4)0.213 (2)0.016 (1)0.5
O420.2003 (10)0.864 (4)0.154 (2)0.016 (1)0.5
O430.1732 (12)0.191 (2)0.2111 (18)0.016 (1)0.5
O440.1803 (13)00.5844 (19)0.016 (1)0.41 (3)
O450.1104 (11)00.648 (3)0.016 (1)0.41 (3)
O460.1762 (12)0.185 (2)0.7047 (19)0.016 (1)0.41 (3)
O470.1953 (13)00.726 (3)0.016 (1)0.59 (3)
O480.1776 (12)00.583 (2)0.016 (1)0.59 (3)
O490.1303 (12)0.188 (2)0.669 (3)0.016 (1)0.59 (3)
O500.2397 (11)00.3421 (18)0.016 (1)0.41 (3)
O510.2642 (13)00.481 (2)0.016 (1)0.41 (3)
O520.1998 (11)0.1918 (16)0.430 (2)0.016 (1)0.41 (3)
O530.1873 (14)00.480 (3)0.016 (1)0.59 (3)
O540.2644 (12)00.478 (3)0.016 (1)0.59 (3)
O550.2186 (10)0.1926 (19)0.3763 (18)0.016 (1)0.59 (3)
O560.4467 (10)00.3284 (15)0.016 (1)
O570.3699 (7)00.268 (2)0.016 (1)
O580.4281 (9)0.179 (2)0.2041 (15)0.016 (1)
O590.4706 (11)00.070 (2)0.016 (1)
O600.4794 (15)00.076 (2)0.016 (1)
O610.5329 (9)0.1844 (17)0.003 (2)0.016 (1)
O620.5126 (10)00.4235 (18)0.016 (1)
O630.4357 (10)00.471 (2)0.016 (1)
O640.4939 (11)0.1927 (19)0.5364 (17)0.016 (1)
O650.5623 (14)00.1528 (18)0.016 (5)0.41 (5)
O660.6162 (10)00.260 (2)0.016 (5)0.41 (5)
O670.5482 (12)0.193 (2)0.272 (2)0.016 (5)0.41 (5)
O680.6030 (10)00.3053 (19)0.016 (5)0.59 (5)
O690.5860 (12)00.1658 (18)0.016 (5)0.59 (5)
O700.5393 (9)0.1866 (17)0.2549 (19)0.016 (5)0.59 (5)
O710.7352 (11)00.1707 (19)0.016 (5)
O720.7138 (10)00.032 (2)0.016 (5)
O730.7815 (10)0.187 (2)0.0832 (19)0.016 (5)
O740.7689 (11)00.507 (2)0.016 (5)
O750.7020 (10)00.579 (2)0.016 (5)
O760.7646 (10)0.1836 (17)0.6330 (19)0.016 (5)
O770.8031 (11)0.092 (5)0.262 (2)0.016 (5)0.5
O780.7934 (13)0.844 (5)0.363 (3)0.016 (5)0.5
O790.8635 (12)0.867 (4)0.315 (2)0.016 (5)0.5
O800.8444 (12)0.123 (4)0.400 (2)0.016 (5)0.5
O810.8038 (11)00.0796 (19)0.016 (5)
O820.8726 (11)00.859 (2)0.016 (5)
O830.8095 (12)0.191 (2)0.7989 (19)0.016 (5)
(Portlandite) top
Crystal data top
CaH2O2Cu Kα1 radiation, λ = 1.5406 Å
Trigonal, P3m1T = 310 K
a = 3.597 Åwhite
c = 4.910 Åflat_sheet, 22 × 22 mm
V = 55.02 Å3Specimen preparation: Prepared at 310 K and 101.325 kPa
Z = 1
Data collection top
D8 Bruker
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tube, KFL CU 2K SiemensScan method: step
None monochromator2θmin = 7.0°, 2θmax = 39.996°, 2θstep = 0.024°
Specimen mounting: temperated sample holder (PMMA) with Kapton film cover
Refinement top
Least-squares matrix: fullProfile function: fundamental parameter type peaks in a non linear least-squares refinement
Rp = 4.29H-atom parameters not defined?
Rwp = 6.06
Rexp = 3.30Background function: combination of Chebychev polynomial 0th order and fundamental parameter type peaks phase
1396 data pointsPreferred orientation correction: spherical harmonics function
Excluded region(s): none
Special details top

Experimental. In-situ experiment with special cooling/heating device for temperature constancy.

Refinement. Portlandite structure from "Busing, W. R., & Levy, H. A. (1986). Neutron diffraction study of calcium hydroxide. Acta Crystallographica B, 42 , 51-55." was used for refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
Ca10000.88
O10.33330.66670.2341 (3)0.797
H10.33330.66670.4248 (6)3.26
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
 

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