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A Refinement of the Crystal Structure of Na2 C0 3 • H2 0

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A Refinement of the Crystal Structure of Na2 C0 3 • H2 0 JOURNAL O F RESEARCH of the National Bureau of Standards - A. Physics and Chemistry Vol. 74A, No. 3, May- June 1970 A Refinement of the Crystal Structure of Na2 C0 3 • H2 0 B. Dickens, F. A. Maue r, and W. E. Brown* Institute for Materi als Research, National Bureau of Standards Washington, D.C. 20234 (January 28, 1970) The c rystal structure of synthe ti c Na2 Co.,,· H2O. has been refin ed us in g 1231 unique x·ray dif· fr~c tlOn data c~ l ec l e d by the peak height m ~ th o d on a diffractomete r. R = 0.034. The unit cell is a - 6.474(2), b- 1O.724(3) and c=5.259(2) A with z = 4 a nd s pace group P2,ab. The calc ulated de nsit y IS the same as the observe d dens it y, 2.26 g. c m- 3 . The structure cont ain s sheets of C0.§- ions bonded to Na+ IOn s a nd water molecul es roughly halfw ay betw een the s heets. Each C02- bonds ed rre· wise to both Na+ ions. The Na+ ions have irregul ar but simila r coordi nations of seve n "' ~ i ghb o r s . Ea~h wa ter molec ule is bonded to both Na+ ions and form s hydrogen bonds to bot h neig hboring Co. ~ - layers. Key words : Crystal struc ture; hyd rated carbonates; hydrogen bonding; sodium carbonate; the rmonatrite; x·ray diffracti on. 1. Introduction of aqueous solution a t 60 °C. Linear absorption coeffi­ cient: 4.37 c m- I . Absorption co rrections: None applied. Maximum error in any intensity from absorption is The crystal structure of Na 2C 0 3 . H 20 was deter· mined except for the hydrogen positions, by Harper - 10 percent. Number of reflections: 2189 were col­ lected from 2 octants and merged into a unique set [1] I in 1936 using qualitative estimates of the x·ray intensities. In our program of studies on coordination of 1231 of which 1132 are "observed" re fl ections and in hydrated carbonates [2] and phosphates [3], we have 99 are less th a n 20- above bac kground and are " un ­ observed". Max imum sin e/ i--. for data.: 0.904 A- I. refin ed Harper's structure for Na2CO:! · H 20 using Method used to estimate data: peak height meas ure­ new x·ray data. Na2CO:1·H 20 is the mineral thermona· trite and often occurs with Na2CO:) . 1OH 20 (natron) ment [8] with a s in gle crys ta l diffractometer [9] and and Na2C03 • NaHC03 • 2H20 (trona) [4,5,6]. some peak heights s tandardized against 8/28 scans. Scattering factors: Na, C, 0 , for neutral atoms give n 2. Determination of the Structure in reference rIO]; H from. reference [Ill Least·squares refin ~ me "ts: Full·mat6x, with !'(wllFol-IFcll)2 mini­ mized. Refine ments include unobserved reflections Formula: Na2 COOl' H 20. Unit ceLL: Orthorhombic with ( a = 6.472(2) A, b = 1O.724(3) A, c=5.259(2) A at 24 °C for which the calculared intensities are more than as calculated from three pairs of 28 values of axial 20- above background. Least·squares weights: 1/0-2 re fl ections from a single crystal and observed on a normalized so that maximum weight is 1. Definitions: diffractometer. The standard deviations of the cell counts in peak = 1= P - (T/2TB ) (BI. + B H ) , 0-(1) parameters are in parentheses and are esti mates based = (P + (BI. + B H ) (T/ (2TB ) )2)1 /2, F = (AF)(LP)(I))I/2, o-(F) = (0-(1)/2) (LP/I) 1/ 2 where P= counts at the gn experience with the technique.o Cell vo lume: 365.1 A3. Wavelength used: 0.710688 A (Mo Ka). Filter: peak position, BI. and Bli = background counts at lower and higher 28 respectively, T= time spent counting 0.025 mm Nb. Space Croup: P2 l ab. CeLL contents in peak, TIJ = time spent counting each background, formula Wts: 4. EqLtivalent positions: x, y, z; 1/2 + x , r -y, -z; 1/2 +x, 1/2-y, z; x, 1/2 +y, -z. Reciprocal AF = attenuator· factor, LP = Lorentz polarization lattice extinctions: hOl, h 7'= 2n; hkO , k 7'= 2n. Observed correction. density: 2.255 g' c m- 3 [7]. Calculated density: 2.256 [ g . cm - 3 . Habit: Fragment from plate. Size of crystal: - 0.35 mm max. - 0.05 mm min. Origin: Evaporation *Di rf'C IOr. Research Associat e Program of the American Dental Associat ion at the National Bureau of S tandar<]s. 1 Fi ~ lI re s in brackets indir' atc the lit erature refe rences at the end (If this pape r. 319 Final R w: 0.029. Final R: 0.032. A verage shift/error sheets at x - 0.25 and x - 0.75. Because the C atoms for last cycle: 0.015. Thermal parameters: anisotropic li e close to the planes of th e a glides, they form columns with form along a at y= 0.25, z - 0.60. Two adjacent C03 groups in a column are held together by both being ionically exp (-I/4(a*2B ll h2+ b*2B22k2+ c*2B33 l 2+ 2a*b*Blzhk bonded to four Na ions and hydrogen bonded by one water molecule. The four Na ions and the water mole­ + 2a*c*B 13hl + 2b *c* B23kL). c ule form a pentagon roughly halfway between the C03 s heets. Adjacent C03 groups in a given sheet The structure was refined isotropically from Harper's are linked by the Na ions that lie above and below parameters using the x-ray 67 system [12] of computer the sheet. programs to Rw=0.065 ; the x parameter of Na(I) was fix ed at x = O. The structure was refin ed ani so­ 3.1. The Carbonate Anion and Invironment tropically to Rw= 0.044 and the hydroge ns were found unambiguously as the two hi ghest peaks in the dif­ The dimensions in the C03 anion are given in table ference synthesis in which the coeffi cients were 4 and the environment is d etailed in table 4 and fi gure weighted by the least squares weights. The two next 2. The C03 group is nearly trigo nal. As can be seen in ) highest peaks were less than 3/4 as high as the peaks fi gures 1 and 2, 0 (2) is the only oxygen which is not assigned to hydrogen s and were (a) halfw\}y, between hydrogen bonded , bein g instead ionically bonded to C and 0(3) in the C03 group and (b) 0.7 A from 0(1) four Na ions. The absence of hydrogen bonding to of the C03 group. The hydrogens were included with 0(2) may account for the observation that the C-0(2) variable pOOiitional parameters and fixed thermal bond is apparently the s hortest of the three. 0 (1) is parameters (BH=I A2) in the final refinement to coordinated to three Na ions and is the acceptor in Rw= 0.029. The largest correlation coeffi cients are the hydrogen bond 0 (1) ... H(I )-0(4) from the - 0.25 between the scale factor and the B II thermal water molecule. 0 (3) is bonq,ed strongly to two Na parameters of the two N a ions and - 0.15 between ions and more weakly (2. 822 A) to a third Na(2). 0(3) these B II thermal parameters. Most correlation coeffi­ is the acceptor in the hydrogen bond 0(3) ... cients are less than 0.05. H(2)-0(4) from the water molecule. The atomic parameters are given in table 1. The Since the planes of the C03 groups are all essen­ observed and calculated structure factors are given in tially perpendicular to a, this is expected to be the table 2. The hydrogen posi ti ons obtained from the direction of lowest refractive index, as was found by weighted difference synthoesis and from the refin e­ Harper [1] . Later workers [1 3, 14] apparently did not ments differ by - 0.17 A. "Calculated" hydrogen permute the refractive indexes when they permuted positions were derived by applying the geometry of the unit cell axes to fit crystallographic convention. free water (0-H=0.958 A, LH-O-H= 104.5°) with the constraint that the o-H . 0 angles be 3.2. The Sodium Environments as near to linear as possible. These hydrogen pq,sitions differ from the other positions by about 0.3 A. The The two crystallographically distinct Na ions in the three sets of hydroge n positions are compared in structure are in general positions. Their environments table 3. The distances and angles which involve are shown in fi gure 3 and are given in table 5. hydrogen were obtained using the "calculated" Na(I) is bonded ionic ally to five oxygens from C0 3 hydrogen positions. groups, and strongly to one water oxygen. Four of the C03 oxygens, 0 (1), 0 (2'), 0(3), 0 (3'), figure 3, define an approximate square about Na(1), and water oxygen 3. Description of the Structure 0(4) forms the apex of a square pyramid. The fifth carbonate oxygen, 0(2), is in the same C0 3 group as The structure (fig. 1) contains C03 anions whose 0 (1); the C03 group is therefore coordinated edgewise planes are almost perpendicular to a and which form to Na(I).
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