Literature DB >> 21582374

Poly[[μ-aqua-aqua-[μ(4)-ethyl (dichloro-methyl-ene)diphospho-nato]sesqui-calcium(II)] acetone hemisolvate 4.5-hydrate].

Jonna Jokiniemi, Sirpa Peräniemi, Jouko Vepsäläinen, Markku Ahlgrén.   

Abstract

The title compound, {[Ca(1.5)(C(3)H(5)Cl(2)O(6)P(2))(H(2)O)(2)]·0.5CH(3)COCH(3)·4.5H(2)O}(n), has a two-dimensional polymeric structure. The asymmetric unit contains two crystallographically independent Ca(2+) cations connected by a chelating and bridging ethyl (dichloro-methyl-ene)diphos-pho-n-ate(3(-)) ligand and an aqua ligand. One of the Ca atoms, lying on a centre of symmetry, has a slightly distorted octa-hedral geometry, while the other Ca atom is seven-coordinated in a distorted monocapped trigonal-prismatic geometry. The polymeric layers are further connected by extensive O-H⋯O hydrogen bonding into a three-dimensional supra-molecular network. The acetone solvent mol-ecule and one uncoordin-ated water mol-ecule are located on twofold rotation axes.

Entities:  

Year:  2009        PMID： 21582374      PMCID： PMC2968796          DOI： 10.1107/S1600536809010150

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For applications of metal complexes of bis­phospho­nates, see: Clearfield et al. (2001 ▶); Clearfield (1998 ▶); Fu et al. (2007 ▶); Serre et al. (2006 ▶). For calcium bis­phospho­nate complexes, see: Lin et al. (2007 ▶); Mathew et al. (1998 ▶). For metal complexes of bis­phospho­nate ester derivatives, see: Jokiniemi et al. (2007 ▶, 2008 ▶).

Experimental

Crystal data

[Ca1.5(C3H5Cl2O6P2)(H2O)2]·0.5C3H6O·4.5H2O M = 476.17 Monoclinic, a = 31.2205 (3) Å b = 10.1546 (1) Å c = 11.6510 (1) Å β = 103.107 (1)° V = 3597.51 (6) Å3 Z = 8 Mo Kα radiation μ = 1.02 mm−1 T = 150 K 0.25 × 0.15 × 0.10 mm

Data collection

Nonius KappaCCD diffractometer Absorption correction: multi-scan (XPREP in SHELXTL; Sheldrick, 2008 ▶) T min = 0.823, T max = 0.905 31118 measured reflections 4209 independent reflections 3617 reflections with I > 2σ(I) R int = 0.055

Refinement

R[F 2 > 2σ(F 2)] = 0.030 wR(F 2) = 0.073 S = 1.10 4209 reflections 213 parameters H-atom parameters constrained Δρmax = 0.47 e Å−3 Δρmin = −0.58 e Å−3 Data collection: COLLECT (Nonius, 1997 ▶); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997 ▶); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2005 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809010150/xu2487sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809010150/xu2487Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ca1.5(C3H5Cl2O6P2)(H2O)2]·0.5C3H6O·4.5H2OF(000) = 1968
Mr = 476.17Dx = 1.758 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 31118 reflections
a = 31.2205 (3) Åθ = 2.7–28.0°
b = 10.1546 (1) ŵ = 1.02 mm−1
c = 11.6510 (1) ÅT = 150 K
β = 103.107 (1)°Needle, colourless
V = 3597.51 (6) Å30.25 × 0.15 × 0.10 mm
Z = 8
Nonius KappaCCD diffractometer4209 independent reflections
Radiation source: fine-focus sealed tube3617 reflections with I > 2σ(I)
graphiteRint = 0.055
φ scans, and ω scans with κ offsetsθmax = 28.0°, θmin = 2.7°
Absorption correction: multi-scan (XPREP in SHELXTL; Sheldrick, 2008)h = −40→40
Tmin = 0.823, Tmax = 0.905k = −13→13
31118 measured reflectionsl = −14→15
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 1.10w = 1/[σ2(Fo2) + (0.02P)2 + 12P] where P = (Fo2 + 2Fc2)/3
4209 reflections(Δ/σ)max = 0.001
213 parametersΔρmax = 0.47 e Å−3
0 restraintsΔρmin = −0.58 e Å−3
Experimental. These results are supported by the IR spectrum and TG analysis. Anal. Found: C, 9.30; H, 3.06%. Calc. for C3H11Cl2Ca1.5O9P2: C, 9.38; H, 2.89%. Main IR absorptions (KBr pellet, cm-1): 3385 (b,s), 2995 (w), 1648 (b,m), 1389 (m), 1213 (s), 1148 (s), 1105 (versus), 1082 (versus), 1048 (m), 1008 (m), 959 (m), 871 (m), 852 (w), 760 (m). 31P CP/MAS NMR: δP 7.4 and 5.1 p.p.m.. TGA (25–700 °C under a synthetic air): 25–180 °C 13.1% (calculated 14.1% for the loss of three water molecules). The observed total weight loss is 40.0% (calculated 41.1% if the final product is assumed to be a mixture of Ca(PO3)2 and CaO in a molar ratio of 2:1).
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/Ueq
Ca10.25000.25000.00000.00999 (12)
Ca20.248223 (14)0.12782 (4)0.36375 (3)0.00930 (9)
Cl10.129792 (17)−0.08747 (5)0.13650 (4)0.01375 (11)
Cl20.137474 (18)0.01918 (5)−0.08762 (4)0.01548 (11)
P10.218448 (17)−0.04904 (5)0.08794 (4)0.00900 (11)
P20.160183 (17)0.18410 (5)0.12307 (5)0.00960 (11)
O10.28281 (5)0.23098 (14)0.20444 (12)0.0126 (3)
H1A0.29110.32170.23180.015*
H1B0.31080.18300.20910.015*
O20.32098 (5)0.03608 (14)0.41612 (13)0.0129 (3)
H2A0.33530.04760.36390.019*
H2B0.3198−0.04670.42440.019*
O30.36311 (5)0.09774 (16)0.24321 (14)0.0178 (3)
H3A0.38990.12150.26830.027*
H3B0.36430.01980.21630.027*
O40.13454 (5)0.36331 (16)0.37057 (14)0.0180 (3)
H4A0.14720.30000.34300.027*
H4B0.15300.38640.43320.027*
O50.05044 (6)0.30916 (18)0.41409 (16)0.0269 (4)
H5A0.07750.31540.41420.040*
H5B0.04760.31180.48510.040*
O60.05040 (6)0.32700 (17)0.66254 (16)0.0238 (4)
H6A0.04050.25790.68830.036*
H6B0.02850.37650.63740.036*
O70.00000.4816 (2)0.25000.0224 (5)
H70.01890.43850.29850.034*
O80.00000.1357 (2)0.75000.0265 (6)
O110.24121 (5)0.03290 (14)0.00999 (12)0.0107 (3)
O120.23607 (5)−0.03674 (14)0.21857 (12)0.0108 (3)
O130.21597 (5)−0.18636 (14)0.04307 (12)0.0103 (3)
O210.18181 (5)0.26929 (14)0.04781 (13)0.0116 (3)
O220.17957 (5)0.18469 (14)0.25168 (12)0.0115 (3)
O230.10987 (5)0.21652 (15)0.10779 (13)0.0132 (3)
C10.16168 (7)0.0176 (2)0.06555 (17)0.0104 (4)
C210.08235 (8)0.2669 (2)0.0003 (2)0.0196 (5)
H21A0.06150.1982−0.03840.024*
H21B0.10060.2944−0.05480.024*
C220.05800 (9)0.3813 (3)0.0325 (3)0.0292 (6)
H22A0.04160.35410.09110.044*
H22B0.03740.4143−0.03800.044*
H22C0.07880.45110.06560.044*
C20.00000.0182 (3)0.75000.0228 (7)
C3−0.02303 (10)−0.0568 (3)0.8273 (3)0.0394 (7)
H3C−0.03170.00330.88370.059*
H3D−0.0033−0.12440.87010.059*
H3E−0.0493−0.09900.77910.059*
U11U22U33U12U13U23
Ca10.0143 (3)0.0066 (3)0.0097 (3)−0.0003 (2)0.0041 (2)0.0006 (2)
Ca20.0130 (2)0.00660 (18)0.00840 (19)−0.00024 (15)0.00261 (15)0.00003 (14)
Cl10.0156 (2)0.0112 (2)0.0157 (3)−0.00233 (19)0.00603 (19)0.00042 (18)
Cl20.0205 (3)0.0151 (2)0.0094 (2)0.0024 (2)0.00041 (19)−0.00142 (18)
P10.0129 (3)0.0059 (2)0.0088 (3)0.00034 (19)0.00368 (19)0.00012 (18)
P20.0122 (3)0.0072 (2)0.0097 (3)0.00102 (19)0.0030 (2)0.00008 (18)
O10.0177 (8)0.0088 (7)0.0112 (7)−0.0003 (6)0.0030 (6)−0.0011 (5)
O20.0160 (7)0.0083 (7)0.0154 (8)−0.0001 (6)0.0054 (6)0.0010 (6)
O30.0171 (8)0.0164 (8)0.0199 (8)0.0005 (6)0.0045 (6)0.0000 (6)
O40.0205 (8)0.0176 (8)0.0152 (8)0.0029 (6)0.0027 (6)−0.0036 (6)
O50.0227 (9)0.0291 (10)0.0296 (10)−0.0008 (8)0.0074 (7)−0.0014 (8)
O60.0200 (9)0.0214 (9)0.0297 (10)−0.0012 (7)0.0053 (7)0.0032 (7)
O70.0205 (12)0.0243 (13)0.0216 (12)0.0000.0032 (10)0.000
O80.0306 (14)0.0174 (12)0.0344 (15)0.0000.0130 (11)0.000
O110.0159 (7)0.0068 (7)0.0109 (7)0.0000 (6)0.0057 (6)0.0007 (5)
O120.0146 (7)0.0086 (7)0.0092 (7)0.0005 (6)0.0027 (6)−0.0010 (5)
O130.0137 (7)0.0072 (7)0.0103 (7)0.0009 (5)0.0030 (6)−0.0011 (5)
O210.0155 (7)0.0068 (7)0.0135 (7)0.0009 (6)0.0052 (6)0.0003 (5)
O220.0146 (7)0.0095 (7)0.0102 (7)0.0017 (6)0.0025 (6)−0.0010 (5)
O230.0130 (7)0.0128 (7)0.0138 (7)0.0040 (6)0.0031 (6)0.0019 (6)
C10.0134 (10)0.0085 (9)0.0095 (10)−0.0008 (8)0.0031 (8)0.0006 (7)
C210.0190 (11)0.0221 (12)0.0155 (11)0.0052 (9)−0.0009 (9)0.0015 (9)
C220.0262 (13)0.0223 (13)0.0356 (15)0.0100 (11)−0.0002 (11)0.0030 (11)
C20.0166 (16)0.0189 (17)0.033 (2)0.0000.0050 (14)0.000
C30.0362 (16)0.0276 (15)0.061 (2)0.0062 (13)0.0253 (15)0.0149 (14)
Ca1—O1i2.3778 (14)P2—O221.4834 (15)
Ca1—O12.3778 (14)P2—O211.4972 (15)
Ca1—O112.2278 (14)P2—O231.5750 (15)
Ca1—O11i2.2278 (14)P2—C11.823 (2)
Ca1—O21i2.3279 (15)O1—H1A0.9900
Ca1—O212.3279 (15)O1—H1B0.9900
Ca1—P2i3.4915 (5)O2—H2A0.8414
Ca1—P23.4915 (5)O2—H2B0.8477
Ca1—P1i3.4204 (5)O3—H3A0.8560
Ca1—P13.4204 (5)O3—H3B0.8554
Ca1—Ca2ii4.1476 (4)O4—H4A0.8541
Ca1—Ca2iii4.1476 (4)O4—H4B0.8536
Ca2—O12.5726 (15)O5—H5A0.8468
Ca2—O22.4024 (15)O5—H5B0.8525
Ca2—O11iv2.4049 (15)O6—H6A0.8481
Ca2—O122.3466 (14)O6—H6B0.8448
Ca2—O13iii2.3320 (15)O7—H70.8416
Ca2—O13iv2.5858 (15)O8—C21.193 (4)
Ca2—O222.3158 (15)O11—Ca2ii2.4049 (15)
Ca2—P1iv3.0705 (6)O13—Ca2vi2.3320 (15)
Ca2—P1iii3.4498 (6)O13—Ca2ii2.5858 (15)
Ca2—P23.4999 (7)O23—C211.442 (3)
Ca2—Ca2v4.0111 (8)C21—C221.482 (3)
Ca2—Ca1vi4.1476 (4)C21—H21A0.9900
Ca2—H2A2.8382C21—H21B0.9900
Ca2—H2B2.8142C22—H22A0.9800
Cl1—C11.785 (2)C22—H22B0.9800
Cl2—C11.773 (2)C22—H22C0.9800
P1—O131.4851 (15)C2—C3vii1.484 (3)
P1—O121.5016 (15)C2—C31.484 (3)
P1—O111.5216 (15)C3—H3C0.9800
P1—C11.860 (2)C3—H3D0.9800
P1—Ca2ii3.0705 (6)C3—H3E0.9800
P1—Ca2vi3.4498 (6)
O21i—Ca1—O21180.00 (6)P2—Ca2—Ca2v114.135 (18)
O21i—Ca1—O1193.40 (5)O22—Ca2—Ca1vi112.14 (4)
O21—Ca1—O1186.60 (5)O13iii—Ca2—Ca1vi127.37 (4)
O21i—Ca1—O11i86.60 (5)O2—Ca2—Ca1vi67.31 (4)
O21—Ca1—O11i93.40 (5)O12—Ca2—Ca1vi66.62 (4)
O11—Ca1—O11i180.00 (8)O11iv—Ca2—Ca1vi25.39 (3)
O21i—Ca1—O1i88.67 (5)O1—Ca2—Ca1vi132.96 (4)
O21—Ca1—O1i91.33 (5)O13iv—Ca2—Ca1vi82.95 (3)
O11—Ca1—O1i95.88 (5)P1iv—Ca2—Ca1vi54.110 (11)
O11i—Ca1—O1i84.12 (5)P1iii—Ca2—Ca1vi147.146 (14)
O21i—Ca1—O191.33 (5)P2—Ca2—Ca1vi113.429 (13)
O21—Ca1—O188.67 (5)Ca2v—Ca2—Ca1vi105.887 (14)
O11—Ca1—O184.12 (5)O22—Ca2—H2A146.7
O11i—Ca1—O195.88 (5)O13iii—Ca2—H2A82.8
O1i—Ca1—O1180.00 (11)O2—Ca2—H2A15.8
O21i—Ca1—P2i19.02 (4)O12—Ca2—H2A78.1
O21—Ca1—P2i160.98 (4)O11iv—Ca2—H2A92.6
O11—Ca1—P2i109.33 (4)O1—Ca2—H2A63.8
O11i—Ca1—P2i70.67 (4)O13iv—Ca2—H2A127.9
O1i—Ca1—P2i77.10 (4)P1iv—Ca2—H2A113.6
O1—Ca1—P2i102.90 (4)P1iii—Ca2—H2A91.1
O21i—Ca1—P2160.98 (4)P2—Ca2—H2A128.7
O21—Ca1—P219.02 (4)Ca2v—Ca2—H2A108.8
O11—Ca1—P270.67 (4)Ca1vi—Ca2—H2A78.7
O11i—Ca1—P2109.33 (4)O22—Ca2—H2B151.6
O1i—Ca1—P2102.90 (4)O13iii—Ca2—H2B97.1
O1—Ca1—P277.10 (4)O2—Ca2—H2B16.4
P2i—Ca1—P2180.000 (18)O12—Ca2—H2B73.8
O21i—Ca1—P1i70.24 (4)O11iv—Ca2—H2B65.8
O21—Ca1—P1i109.76 (4)O1—Ca2—H2B89.9
O11—Ca1—P1i160.29 (4)O13iv—Ca2—H2B112.0
O11i—Ca1—P1i19.71 (4)P1iv—Ca2—H2B89.9
O1i—Ca1—P1i73.49 (4)P1iii—Ca2—H2B111.4
O1—Ca1—P1i106.51 (4)P2—Ca2—H2B137.6
P2i—Ca1—P1i52.709 (12)Ca2v—Ca2—H2B108.2
P2—Ca1—P1i127.291 (12)Ca1vi—Ca2—H2B51.7
O21i—Ca1—P1109.76 (4)H2A—Ca2—H2B27.5
O21—Ca1—P170.24 (4)O13—P1—O12114.38 (8)
O11—Ca1—P119.71 (4)O13—P1—O11107.30 (8)
O11i—Ca1—P1160.29 (4)O12—P1—O11116.49 (8)
O1i—Ca1—P1106.51 (4)O13—P1—C1108.70 (9)
O1—Ca1—P173.49 (4)O12—P1—C1103.32 (9)
P2i—Ca1—P1127.291 (12)O11—P1—C1106.05 (9)
P2—Ca1—P152.709 (12)O13—P1—Ca2ii57.15 (6)
P1i—Ca1—P1180.000 (17)O12—P1—Ca2ii140.52 (6)
O21i—Ca1—Ca2ii76.36 (4)O11—P1—Ca2ii50.37 (6)
O21—Ca1—Ca2ii103.64 (4)C1—P1—Ca2ii116.00 (7)
O11—Ca1—Ca2ii27.57 (4)O12—P1—Ca2vi83.46 (6)
O11i—Ca1—Ca2ii152.43 (4)O11—P1—Ca2vi116.94 (6)
O1i—Ca1—Ca2ii74.12 (4)C1—P1—Ca2vi127.72 (7)
O1—Ca1—Ca2ii105.88 (4)Ca2ii—P1—Ca2vi75.679 (16)
P2i—Ca1—Ca2ii87.845 (10)O13—P1—Ca1136.36 (6)
P2—Ca1—Ca2ii92.155 (10)O12—P1—Ca199.53 (6)
P1i—Ca1—Ca2ii133.342 (10)C1—P1—Ca187.98 (6)
P1—Ca1—Ca2ii46.658 (10)Ca2ii—P1—Ca179.232 (14)
O21i—Ca1—Ca2iii103.64 (4)Ca2vi—P1—Ca1142.808 (18)
O21—Ca1—Ca2iii76.36 (4)O22—P2—O21117.03 (9)
O11—Ca1—Ca2iii152.43 (4)O22—P2—O23106.35 (8)
O11i—Ca1—Ca2iii27.57 (4)O21—P2—O23112.56 (8)
O1i—Ca1—Ca2iii105.88 (4)O22—P2—C1109.66 (9)
O1—Ca1—Ca2iii74.12 (4)O21—P2—C1105.54 (9)
P2i—Ca1—Ca2iii92.155 (10)O23—P2—C1105.09 (9)
P2—Ca1—Ca2iii87.845 (10)O22—P2—Ca1103.43 (6)
P1i—Ca1—Ca2iii46.658 (10)O23—P2—Ca1141.89 (6)
P1—Ca1—Ca2iii133.342 (10)C1—P2—Ca186.38 (7)
Ca2ii—Ca1—Ca2iii180.000 (14)O21—P2—Ca2100.78 (6)
O22—Ca2—O13iii110.21 (5)O23—P2—Ca2134.96 (6)
O22—Ca2—O2160.19 (5)C1—P2—Ca293.57 (7)
O13iii—Ca2—O282.51 (5)Ca1—P2—Ca278.603 (13)
O22—Ca2—O1278.08 (5)Ca1—O1—Ca2126.86 (6)
O13iii—Ca2—O12153.36 (5)Ca1—O1—H1A105.6
O2—Ca2—O1284.02 (5)Ca2—O1—H1A105.6
O22—Ca2—O11iv110.33 (5)Ca1—O1—H1B105.6
O13iii—Ca2—O11iv109.29 (5)Ca2—O1—H1B105.6
O2—Ca2—O11iv77.85 (5)H1A—O1—H1B106.1
O12—Ca2—O11iv90.09 (5)Ca2—O2—H2A112.9
O22—Ca2—O188.74 (5)Ca2—O2—H2B110.5
O13iii—Ca2—O176.76 (5)H2A—O2—H2B105.3
O2—Ca2—O179.26 (5)H3A—O3—H3B105.4
O12—Ca2—O178.20 (5)H4A—O4—H4B104.4
O11iv—Ca2—O1155.24 (5)H5A—O5—H5B108.6
O22—Ca2—O13iv85.30 (5)H6A—O6—H6B106.6
O13iii—Ca2—O13iv70.81 (6)P1—O11—Ca1130.70 (8)
O2—Ca2—O13iv113.76 (5)P1—O11—Ca2ii100.46 (7)
O12—Ca2—O13iv135.83 (5)Ca1—O11—Ca2ii127.05 (6)
O11iv—Ca2—O13iv57.92 (5)P1—O12—Ca2138.76 (9)
O1—Ca2—O13iv142.51 (5)P1—O13—Ca2vi127.93 (8)
O22—Ca2—P1iv97.16 (4)P1—O13—Ca2ii94.01 (7)
O13iii—Ca2—P1iv91.17 (4)Ca2vi—O13—Ca2ii109.19 (6)
O2—Ca2—P1iv97.71 (4)P2—O21—Ca1130.53 (8)
O12—Ca2—P1iv113.39 (4)P2—O22—Ca2133.01 (9)
O11iv—Ca2—P1iv29.16 (3)C21—O23—P2123.71 (14)
O1—Ca2—P1iv167.82 (4)Cl2—C1—Cl1108.43 (11)
O13iv—Ca2—P1iv28.85 (3)Cl2—C1—P1108.63 (11)
O22—Ca2—P1iii93.51 (4)Cl1—C1—P1109.34 (11)
O13iii—Ca2—P1iii19.85 (4)Cl2—C1—P2108.74 (11)
O2—Ca2—P1iii95.43 (4)Cl1—C1—P2108.71 (11)
O12—Ca2—P1iii142.04 (4)P1—C1—P2112.90 (11)
O11iv—Ca2—P1iii127.05 (4)O23—C21—C22107.30 (19)
O1—Ca2—P1iii64.53 (3)O23—C21—H21A110.3
O13iv—Ca2—P1iii78.92 (3)C22—C21—H21A110.3
P1iv—Ca2—P1iii104.321 (16)O23—C21—H21B110.3
O22—Ca2—P218.06 (4)C22—C21—H21B110.3
O13iii—Ca2—P2116.57 (4)H21A—C21—H21B108.5
O2—Ca2—P2142.41 (4)C21—C22—H22A109.5
O12—Ca2—P264.50 (4)C21—C22—H22B109.5
O11iv—Ca2—P2119.83 (4)H22A—C22—H22B109.5
O1—Ca2—P274.77 (4)C21—C22—H22C109.5
O13iv—Ca2—P2103.35 (3)H22A—C22—H22C109.5
P1iv—Ca2—P2112.947 (18)H22B—C22—H22C109.5
P1iii—Ca2—P297.378 (15)O8—C2—C3vii120.89 (17)
O22—Ca2—Ca2v98.51 (4)O8—C2—C3120.89 (17)
O13iii—Ca2—Ca2v37.50 (4)C3vii—C2—C3118.2 (3)
O2—Ca2—Ca2v100.60 (4)C2—C3—H3C109.5
O12—Ca2—Ca2v169.12 (4)C2—C3—H3D109.5
O11iv—Ca2—Ca2v81.36 (4)H3C—C3—H3D109.5
O1—Ca2—Ca2v112.23 (4)C2—C3—H3E109.5
O13iv—Ca2—Ca2v33.30 (3)H3C—C3—H3E109.5
P1iv—Ca2—Ca2v56.443 (13)H3D—C3—H3E109.5
P1iii—Ca2—Ca2v47.877 (12)
D—H···AD—HH···AD···AD—H···A
O1—H1B···O30.991.812.794 (2)171
O1—H1A···O12iii0.991.832.637 (2)137
O2—H2A···O30.841.882.717 (2)172
O2—H2B···O21vi0.851.902.746 (2)177
O3—H3A···O6v0.861.932.782 (2)175
O3—H3B···O4vi0.861.892.734 (2)169
O4—H4A···O220.852.002.841 (2)166
O4—H4B···O2v0.851.932.754 (2)163
O5—H5A···O40.852.022.838 (2)163
O5—H5B···O60.852.052.901 (3)171
O6—H6A···O80.852.022.831 (2)161
O6—H6B···O7viii0.842.262.832 (2)125
O7—H7···O50.841.982.799 (2)166
Table 1

Selected bond lengths (Å)

Ca1—O12.3778 (14)
Ca1—O112.2278 (14)
Ca1—O212.3279 (15)
Ca2—O12.5726 (15)
Ca2—O22.4024 (15)
Ca2—O11i2.4049 (15)
Ca2—O122.3466 (14)
Ca2—O13ii2.3320 (15)
Ca2—O13i2.5858 (15)
Ca2—O222.3158 (15)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1B⋯O30.991.812.794 (2)171
O1—H1A⋯O12ii0.991.832.637 (2)137
O2—H2A⋯O30.841.882.717 (2)172
O2—H2B⋯O21iii0.851.902.746 (2)177
O3—H3A⋯O6iv0.861.932.782 (2)175
O3—H3B⋯O4iii0.861.892.734 (2)169
O4—H4A⋯O220.852.002.841 (2)166
O4—H4B⋯O2iv0.851.932.754 (2)163
O5—H5A⋯O40.852.022.838 (2)163
O5—H5B⋯O60.852.052.901 (3)171
O6—H6A⋯O80.852.022.831 (2)161
O6—H6B⋯O7v0.842.262.832 (2)125
O7—H7⋯O50.841.982.799 (2)166

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) .

  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Synthesis, Characterization, and Crystal Structure of Dicalcium Glutarylbis(phosphonate) Dihydrate: A Covalently Pillared Layer Structure with the Potential for Epitaxial Growth on Hydroxyapatite.

Authors:  Mathai Mathew; Bruce O. Fowler; Eli Breuer; Gershon Golomb; Ivan S. Alferiev; Naomi Eidelman
Journal:  Inorg Chem       Date:  1998-12-14       Impact factor: 5.165
  2 in total

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