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The crystal structure of the inclusion complex of β-cyclo-dextrin with mefenamic acid has been determined from a combination of high-resolution synchrotron powder-diffraction data and molecular-mechanics calculations. A grid search indicates two possible solutions, which are corroborated by molecular-mechanics calculations, while Rietveld-refinement results suggest the crystal structure that is more likely to be formed in the solid state. Mefenamic acid is partially included in β-cyclodextrin with either the xylyl or the benzoic-acid moiety being inside its cavity. In both solutions mefenamic acid and β-cyclodextrin form a monomeric complex in a herringbone packing scheme.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810201947X/na0142sup1.cif
Contains datablocks global, 1, 2

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810201947X/na01421sup2.rtv
Contains datablock 1

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810201947X/na01422sup3.rtv
Contains datablock 2

CCDC references: 201625; 201626

Computing details top

For both compounds, cell refinement: MRIA; data reduction: MRIA; program(s) used to solve structure: MRIA; program(s) used to refine structure: GSAS; molecular graphics: DIAMOND.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(1) β-cyclodextrin mefenamic acid inclusion complex top
Crystal data top
C55.5H13.5N0.9O36.8V = 3637.7 (4) Å3
Mr = 1281.59Z = 2
Monoclinic, P_21Dx = 1.17 Mg m3
Hall symbol: p_2ybSynchrotron radiation, λ = 0.800807 Å
a = 15.4797 (9) ÅT = 295 K
b = 25.5892 (15) Åwhite
c = 9.2973 (5) Åcylinder, ? × 1 mm
β = 98.976 (7)°
Data collection top
ESRF BM16
diffractometer
Data collection mode: transmission
Si(111) double monochromatorScan method: continuous
Specimen mounting: packed powder pellet2θmin = 3.205°, 2θmax = 39.995°, 2θstep = 0.005°
Refinement top
Rp = 0.0987359 data points
Rwp = 0.133141 parameters
Rexp = 0.024126 restraints
χ2 = 36.966(Δ/σ)max = 0.32
Crystal data top
C55.5H13.5N0.9O36.8β = 98.976 (7)°
Mr = 1281.59V = 3637.7 (4) Å3
Monoclinic, P_21Z = 2
a = 15.4797 (9) ÅSynchrotron radiation, λ = 0.800807 Å
b = 25.5892 (15) ÅT = 295 K
c = 9.2973 (5) Åcylinder, ? × 1 mm
Data collection top
ESRF BM16
diffractometer
Scan method: continuous
Specimen mounting: packed powder pellet2θmin = 3.205°, 2θmax = 39.995°, 2θstep = 0.005°
Data collection mode: transmission
Refinement top
Rp = 0.0987359 data points
Rwp = 0.133141 parameters
Rexp = 0.024126 restraints
χ2 = 36.966(Δ/σ)max = 0.32
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1G10.0570 (12)0.7512 (6)0.001 (3)0.09499*
C2G10.1006 (11)0.7500 (6)0.139 (3)0.09499*
C3G10.1998 (11)0.7451 (6)0.114 (3)0.09499*
C4G10.2451 (11)0.7693 (6)0.028 (3)0.09499*
C5G10.1918 (18)0.7644 (6)0.154 (2)0.09499*
O2G10.0594 (15)0.7162 (7)0.250 (3)0.09052*
O3G10.2367 (17)0.7629 (6)0.236 (3)0.09052*
O5G10.1044 (17)0.7832 (6)0.112 (3)0.09052*
O6G10.179 (3)0.7857 (15)0.414 (4)0.09052*
C6G10.197 (3)0.8046 (13)0.278 (3)0.09499*
O4G10.3278 (13)0.7428 (7)0.058 (4)0.09052*
C1G20.1581 (15)0.6349 (8)0.309 (2)0.09499*
C2G20.2078 (11)0.6455 (8)0.154 (3)0.09499*
C3G20.1508 (14)0.6687 (7)0.051 (2)0.09499*
C4G20.0736 (13)0.7010 (7)0.125 (3)0.09499*
C5G20.0499 (14)0.6997 (7)0.293 (3)0.09499*
O2G20.2583 (11)0.6024 (8)0.092 (3)0.09052*
O3G20.2022 (18)0.6989 (8)0.060 (2)0.09052*
O5G20.1192 (18)0.6827 (8)0.368 (2)0.09052*
O6G20.051 (3)0.7370 (14)0.491 (6)0.09052*
C6G20.027 (4)0.7475 (13)0.390 (5)0.09499*
O4G20.0106 (19)0.7175 (12)0.035 (4)0.09052*
C1G30.0431 (11)0.4600 (7)0.473 (2)0.09499*
C2G30.1106 (8)0.4520 (7)0.3335 (18)0.09499*
C3G30.1182 (10)0.5023 (7)0.2450 (19)0.09499*
C4G30.1312 (10)0.5508 (8)0.335 (2)0.09499*
C5G30.0771 (11)0.5501 (8)0.489 (2)0.09499*
O2G30.0897 (8)0.4077 (7)0.2530 (17)0.09052*
O3G30.1782 (15)0.4993 (8)0.113 (2)0.09052*
O5G30.0718 (15)0.5005 (8)0.561 (2)0.09052*
O6G30.194 (3)0.6068 (12)0.550 (3)0.09052*
C6G30.159 (2)0.5560 (13)0.566 (5)0.09499*
O4G30.1000 (19)0.5956 (9)0.267 (4)0.09052*
C1G40.2500 (11)0.4167 (9)0.827 (2)0.09499*
C2G40.2004 (10)0.3679 (8)0.7605 (18)0.09499*
C3G40.1185 (12)0.3825 (7)0.6557 (15)0.09499*
C4G40.0657 (13)0.4257 (8)0.714 (2)0.09499*
C5G40.1205 (14)0.4681 (8)0.8008 (17)0.09499*
O2G40.2558 (9)0.3327 (9)0.701 (3)0.09052*
O3G40.0654 (10)0.3384 (8)0.6076 (18)0.09052*
O5G40.1927 (12)0.4478 (8)0.8996 (17)0.09052*
O6G40.025 (2)0.5318 (14)0.925 (5)0.09052*
C6G40.068 (3)0.4817 (15)0.926 (4)0.09499*
O4G40.0312 (18)0.4299 (12)0.562 (2)0.09052*
C1G50.5675 (10)0.5032 (7)0.6798 (16)0.09499*
C2G50.5694 (8)0.4430 (7)0.6895 (19)0.09499*
C3G50.4794 (8)0.4187 (7)0.6830 (14)0.09499*
C4G50.4234 (11)0.4484 (8)0.777 (2)0.09499*
C5G50.4325 (10)0.5079 (8)0.765 (3)0.09499*
O2G50.6226 (9)0.4200 (8)0.595 (3)0.09052*
O3G50.4855 (11)0.3646 (7)0.7180 (16)0.09052*
O5G50.5212 (10)0.5247 (7)0.7869 (17)0.09052*
O6G50.3651 (18)0.6090 (11)0.794 (5)0.09052*
C6G50.372 (3)0.5526 (11)0.818 (7)0.09499*
O4G50.3351 (14)0.4249 (12)0.771 (4)0.09052*
C1G60.5754 (7)0.6684 (6)0.278 (3)0.09499*
C2G60.5828 (8)0.6156 (6)0.199 (3)0.09499*
C3G60.5376 (6)0.5714 (5)0.269 (2)0.09499*
C4G60.5577 (11)0.5716 (6)0.434 (2)0.09499*
C5G60.5648 (15)0.6261 (7)0.504 (3)0.09499*
O2G60.5559 (15)0.6199 (7)0.046 (3)0.09052*
O3G60.5597 (7)0.5210 (6)0.222 (2)0.09052*
O5G60.6110 (10)0.6632 (6)0.429 (3)0.09052*
O6G60.658 (2)0.5864 (14)0.654 (5)0.09052*
C6G60.602 (3)0.6290 (19)0.667 (3)0.09499*
O4G60.566 (2)0.5306 (10)0.542 (2)0.09052*
C1G70.3575 (11)0.7956 (5)0.064 (3)0.09499*
C2G70.4195 (12)0.7858 (6)0.049 (3)0.09499*
C3G70.4818 (11)0.7402 (6)0.004 (2)0.09499*
C4G70.5100 (12)0.7319 (6)0.159 (3)0.09499*
C5G70.4521 (16)0.7579 (6)0.259 (3)0.09499*
O2G70.3738 (16)0.7805 (7)0.193 (3)0.09052*
O3G70.5536 (13)0.7376 (6)0.082 (3)0.09052*
O5G70.4084 (15)0.8047 (6)0.205 (3)0.09052*
O6G70.474 (3)0.7358 (12)0.495 (5)0.09052*
C6G70.418 (2)0.7205 (10)0.366 (4)0.09499*
O4G70.4880 (11)0.6852 (7)0.231 (3)0.09052*
O10.1888 (19)0.3904 (13)0.151 (4)0.09052*.90000
O20.290 (2)0.3275 (11)0.2744 (18)0.09052*.90000
N30.2959 (18)0.4791 (12)0.130 (4)0.09499*.90000
C40.3641 (15)0.4418 (11)0.170 (4)0.09499*.90000
C50.4546 (13)0.4492 (6)0.172 (4)0.09499*.90000
C60.5318 (8)0.4243 (7)0.240 (4)0.09499*.90000
C70.5150 (12)0.3742 (7)0.295 (4)0.09499*.90000
C80.4271 (14)0.3579 (9)0.274 (3)0.09499*.90000
C90.3556 (16)0.3895 (11)0.213 (4)0.09499*.90000
C100.2636 (16)0.3707 (13)0.211 (4)0.09499*.90000
C110.263 (2)0.5309 (11)0.143 (3)0.09499*.90000
C120.263 (2)0.5368 (10)0.294 (3)0.09499*.90000
C130.239 (2)0.5850 (14)0.3497 (17)0.09499*.90000
C140.210 (2)0.6248 (8)0.251 (3)0.09499*.90000
C150.211 (2)0.6216 (10)0.102 (3)0.09499*.90000
C160.241 (2)0.5749 (11)0.049 (3)0.09499*.90000
C170.2362 (11)0.5704 (5)0.112 (3)0.09499*.90000
C180.1879 (8)0.6704 (7)0.0125 (17)0.09499*.90000
H190.257090.462880.051940.10000*.90000
H200.276620.508570.364230.10000*.90000
H210.230040.587780.451240.10000*.90000
H220.198330.657690.292470.10000*.90000
H230.143230.659280.071130.10000*.90000
H240.241970.678970.025680.10000*.90000
H250.170140.698230.078690.10000*.90000
H260.186610.581980.160750.10000*.90000
H270.234810.532300.123420.10000*.90000
H280.294630.579980.127010.10000*.90000
H290.467420.485000.151890.10000*.90000
H300.593950.429650.251430.10000*.90000
H310.552410.344900.324190.10000*.90000
H320.407090.328980.326400.10000*.90000
H330.282540.336620.377350.10000*.90000
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
Geometric parameters (Å, º) top
C1G1—O5G11.43 (3)C5G5—C6G51.60 (5)
C1G1—O4G21.43 (4)O6G5—C6G51.46 (4)
C1G1—C2G11.56 (4)C1G6—O4G71.42 (2)
C2G1—O2G11.42 (3)C1G6—O5G61.43 (4)
C2G1—C3G11.52 (2)C1G6—C2G61.55 (3)
C3G1—O3G11.42 (4)C2G6—O2G61.42 (4)
C3G1—C4G11.53 (3)C2G6—C3G61.53 (2)
C4G1—O4G11.44 (3)C3G6—O3G61.42 (2)
C4G1—C5G11.54 (4)C3G6—C4G61.52 (3)
C5G1—O5G11.43 (4)C4G6—O4G61.44 (3)
C5G1—C6G11.54 (4)C4G6—C5G61.54 (3)
O6G1—C6G11.42 (5)C5G6—O5G61.43 (3)
O4G1—C1G71.43 (2)C5G6—C6G61.54 (4)
C1G2—O5G21.43 (3)O6G6—C6G61.41 (6)
C1G2—O4G31.44 (4)C1G7—O5G71.44 (3)
C1G2—C2G21.55 (3)C1G7—C2G71.55 (4)
C2G2—O2G21.42 (3)C2G7—O2G71.42 (4)
C2G2—C3G21.52 (3)C2G7—C3G71.53 (2)
C3G2—O3G21.43 (3)C3G7—O3G71.42 (3)
C3G2—C4G21.53 (3)C3G7—C4G71.53 (3)
C4G2—O4G21.44 (4)C4G7—O4G71.44 (3)
C4G2—C5G21.55 (4)C4G7—C5G71.54 (4)
C5G2—O5G21.44 (4)C5G7—O5G71.43 (3)
C5G2—C6G21.53 (4)C5G7—C6G71.53 (4)
O6G2—C6G21.43 (7)O6G7—C6G71.42 (5)
C1G3—O5G31.43 (3)O1—C101.31 (4)
C1G3—O4G41.52 (3)O2—H331.01 (2)
C1G3—C2G31.55 (2)O2—C101.29 (4)
C2G3—O2G31.42 (2)N3—H190.96 (3)
C2G3—C3G31.52 (2)N3—C41.43 (4)
C3G3—O3G31.42 (2)N3—C111.43 (4)
C3G3—C4G31.53 (3)C4—C91.41 (4)
C4G3—O4G31.43 (3)C4—C51.41 (3)
C4G3—C5G31.54 (2)C5—H290.962 (18)
C5G3—O5G31.43 (3)C5—C61.41 (3)
C5G3—C6G31.56 (4)C6—H300.961 (13)
O6G3—C6G31.41 (5)C6—C71.42 (3)
C1G4—O5G41.44 (3)C7—H310.960 (19)
C1G4—O4G51.50 (3)C7—C81.41 (3)
C1G4—C2G41.54 (3)C8—H320.96 (3)
C2G4—O2G41.41 (3)C8—C91.42 (3)
C2G4—C3G41.52 (2)C9—C101.50 (4)
C3G4—O3G41.43 (3)C11—C121.41 (4)
C3G4—C4G41.52 (3)C11—C161.43 (4)
C4G4—O4G41.43 (3)C12—H200.97 (3)
C4G4—C5G41.53 (3)C12—C131.41 (4)
C5G4—O5G41.43 (2)C13—H210.978 (18)
C5G4—C6G41.56 (5)C13—C141.40 (4)
O6G4—C6G41.44 (5)C14—H220.95 (2)
C1G5—O5G51.42 (2)C14—C151.39 (4)
C1G5—O4G61.46 (3)C15—C161.40 (4)
C1G5—C2G51.54 (3)C15—C181.51 (3)
C2G5—O2G51.42 (3)C16—C171.49 (4)
C2G5—C3G51.52 (2)C17—H260.880 (18)
C3G5—O3G51.42 (3)C17—H280.968 (18)
C3G5—C4G51.53 (2)C17—H270.980 (13)
C4G5—O4G51.49 (3)C18—H240.984 (14)
C4G5—C5G51.53 (3)C18—H230.998 (14)
C5G5—O5G51.42 (2)C18—H251.007 (17)
O5G1—C1G1—O4G2120 (3)O4G7—C1G6—C2G6104.8 (15)
O5G1—C1G1—C2G1112.0 (18)O5G6—C1G6—C2G6109.7 (15)
O4G2—C1G1—C2G1127 (2)O2G6—C2G6—C3G6113.6 (15)
O2G1—C2G1—C3G1113 (2)O2G6—C2G6—C1G6112.0 (16)
O2G1—C2G1—C1G1114.6 (17)C3G6—C2G6—C1G6111.8 (19)
C3G1—C2G1—C1G1116 (2)O3G6—C3G6—C4G6107.0 (13)
O3G1—C3G1—C2G1112 (2)O3G6—C3G6—C2G6113.1 (14)
O3G1—C3G1—C4G1111.9 (16)C4G6—C3G6—C2G6113.1 (14)
C2G1—C3G1—C4G1115 (2)O4G6—C4G6—C3G6133.1 (15)
O4G1—C4G1—C3G1105 (2)O4G6—C4G6—C5G6111.9 (18)
O4G1—C4G1—C5G1112 (2)C3G6—C4G6—C5G6114.9 (15)
C3G1—C4G1—C5G1113.4 (16)O5G6—C5G6—C4G6114 (2)
O5G1—C5G1—C6G185 (2)O5G6—C5G6—C6G6108 (2)
O5G1—C5G1—C4G1111.2 (18)C4G6—C5G6—C6G6117 (2)
C6G1—C5G1—C4G1123 (2)C1G6—O5G6—C5G6113.2 (16)
C1G1—O5G1—C5G1111.2 (17)O6G6—C6G6—C5G691 (3)
O6G1—C6G1—C5G1116 (3)C4G6—O4G6—C1G5161 (2)
C1G7—O4G1—C4G180.3 (13)O4G1—C1G7—O5G7108 (2)
O5G2—C1G2—O4G3117 (2)O4G1—C1G7—C2G792.9 (18)
O5G2—C1G2—C2G2108.9 (16)O5G7—C1G7—C2G7109.6 (17)
O4G3—C1G2—C2G296 (2)O2G7—C2G7—C3G7112.7 (17)
O2G2—C2G2—C3G2113 (2)O2G7—C2G7—C1G7112.6 (18)
O2G2—C2G2—C1G2114 (2)C3G7—C2G7—C1G7111.6 (18)
C3G2—C2G2—C1G2113.7 (15)O3G7—C3G7—C4G7112.0 (16)
O3G2—C3G2—C2G2111 (2)O3G7—C3G7—C2G7114.0 (17)
O3G2—C3G2—C4G2110.0 (17)C4G7—C3G7—C2G7116.6 (17)
C2G2—C3G2—C4G2114.7 (18)O4G7—C4G7—C3G7121.8 (17)
O4G2—C4G2—C3G2117 (2)O4G7—C4G7—C5G782.8 (18)
O4G2—C4G2—C5G2121 (2)C3G7—C4G7—C5G7115.9 (16)
C3G2—C4G2—C5G2119.3 (19)O5G7—C5G7—C6G7124 (2)
O5G2—C5G2—C6G294 (3)O5G7—C5G7—C4G7116 (2)
O5G2—C5G2—C4G2114.8 (18)C6G7—C5G7—C4G7114.5 (17)
C6G2—C5G2—C4G2125 (2)C5G7—O5G7—C1G7110.3 (17)
C1G2—O5G2—C5G2111.9 (19)O6G7—C6G7—C5G799 (3)
O6G2—C6G2—C5G2109 (3)C1G6—O4G7—C4G796.4 (15)
C1G1—O4G2—C4G2153 (3)H33—O2—C1099 (3)
O5G3—C1G3—O4G4109.4 (16)H19—N3—C4105 (3)
O5G3—C1G3—C2G3110.2 (15)H19—N3—C11106 (3)
O4G4—C1G3—C2G3138.2 (17)C4—N3—C11149 (3)
O2G3—C2G3—C3G3113.2 (15)C9—C4—C5105 (2)
O2G3—C2G3—C1G3111.5 (12)C9—C4—N3128 (2)
C3G3—C2G3—C1G3109.1 (13)C5—C4—N3127 (3)
O3G3—C3G3—C2G3114.0 (15)H29—C5—C4111.1 (19)
O3G3—C3G3—C4G3113.1 (15)H29—C5—C6109.3 (18)
C2G3—C3G3—C4G3113.4 (15)C4—C5—C6136 (3)
O4G3—C4G3—C3G3109 (2)H30—C6—C5138 (2)
O4G3—C4G3—C5G3104.4 (18)H30—C6—C7109.0 (17)
C3G3—C4G3—C5G3113.6 (15)C5—C6—C7112.3 (14)
O5G3—C5G3—C4G3115.3 (16)H31—C7—C8109.6 (18)
O5G3—C5G3—C6G382.1 (19)H31—C7—C6132 (2)
C4G3—C5G3—C6G393.6 (18)C8—C7—C6116.4 (18)
C5G3—O5G3—C1G3112.0 (17)H32—C8—C7123 (2)
O6G3—C6G3—C5G3112 (3)H32—C8—C9110 (2)
C4G3—O4G3—C1G2100 (2)C7—C8—C9124 (2)
O5G4—C1G4—O4G5136 (2)C4—C9—C8124 (2)
O5G4—C1G4—C2G4109.4 (15)C4—C9—C10116 (2)
O4G5—C1G4—C2G4112 (2)C8—C9—C10120 (3)
O2G4—C2G4—C3G4113.7 (16)O2—C10—O1136 (3)
O2G4—C2G4—C1G4112.2 (14)O2—C10—C992 (2)
C3G4—C2G4—C1G4111.8 (16)O1—C10—C9131 (3)
O3G4—C3G4—C2G4112.9 (15)C12—C11—N3104 (3)
O3G4—C3G4—C4G4111.8 (16)C12—C11—C16119 (3)
C2G4—C3G4—C4G4113.0 (13)N3—C11—C16137 (3)
O4G4—C4G4—C3G480.9 (16)H20—C12—C13116 (3)
O4G4—C4G4—C5G4124 (2)H20—C12—C11124 (3)
C3G4—C4G4—C5G4114.7 (16)C13—C12—C11120 (2)
O5G4—C5G4—C4G4113.3 (17)H21—C13—C14120 (3)
O5G4—C5G4—C6G492.7 (18)H21—C13—C12120 (3)
C4G4—C5G4—C6G4104 (2)C14—C13—C12118 (2)
C5G4—O5G4—C1G4112.2 (15)H22—C14—C15119 (2)
O6G4—C6G4—C5G4119 (3)H22—C14—C13116 (3)
C4G4—O4G4—C1G3135 (2)C15—C14—C13124 (2)
O5G5—C1G5—O4G6119.2 (17)C14—C15—C16117 (2)
O5G5—C1G5—C2G5110.6 (14)C14—C15—C18117 (2)
O4G6—C1G5—C2G5122.0 (16)C16—C15—C18125 (2)
O2G5—C2G5—C3G5115.0 (14)C15—C16—C11121 (3)
O2G5—C2G5—C1G5112.6 (15)C15—C16—C17117 (2)
C3G5—C2G5—C1G5113.4 (12)C11—C16—C17121 (2)
O3G5—C3G5—C2G5111.2 (13)H26—C17—H28127 (3)
O3G5—C3G5—C4G5112.2 (14)H26—C17—H27106.1 (17)
C2G5—C3G5—C4G5111.9 (14)H26—C17—C16113 (2)
O4G5—C4G5—C3G5112.2 (19)H28—C17—H27104.0 (16)
O4G5—C4G5—C5G5119.5 (17)H28—C17—C16103 (2)
C3G5—C4G5—C5G5112.7 (16)H27—C17—C16101 (2)
O5G5—C5G5—C4G5112.8 (15)H24—C18—H23107.9 (15)
O5G5—C5G5—C6G5110 (2)H24—C18—H25113.1 (16)
C4G5—C5G5—C6G5128 (2)H24—C18—C15104.0 (16)
C5G5—O5G5—C1G5111.3 (16)H23—C18—H25117.1 (13)
O6G5—C6G5—C5G5134 (4)H23—C18—C15105.6 (17)
C4G5—O4G5—C1G4153 (3)H25—C18—C15108.1 (17)
O4G7—C1G6—O5G6122 (2)
O5G1—C1G1—C2G1—C3G142 (2)C4G5—C5G5—O5G5—C1G561 (2)
O5G1—C1G1—C2G1—O2G1176.3 (16)C6G5—C5G5—O5G5—C1G5149 (3)
O4G2—C1G1—C2G1—C3G1125 (2)C4G5—C5G5—C6G5—O6G5169 (4)
O4G2—C1G1—C2G1—O2G19 (3)O5G5—C5G5—C6G5—O6G547 (6)
C2G1—C1G1—O5G1—C5G160 (2)O5G6—C1G6—C2G6—C3G656.7 (15)
O4G2—C1G1—O5G1—C5G1108 (3)O5G6—C1G6—C2G6—O2G6174.5 (16)
C2G1—C1G1—O4G2—C4G2175 (4)O4G7—C1G6—C2G6—C3G676 (2)
O5G1—C1G1—O4G2—C4G219 (6)O4G7—C1G6—C2G6—O2G653 (2)
C1G1—C2G1—C3G1—C4G130 (2)C2G6—C1G6—O5G6—C5G662 (2)
C1G1—C2G1—C3G1—O3G1158.7 (15)O4G7—C1G6—O5G6—C5G661 (2)
O2G1—C2G1—C3G1—C4G1164.7 (18)C2G6—C1G6—O4G7—C4G7117 (2)
O2G1—C2G1—C3G1—O3G167 (2)O5G6—C1G6—O4G7—C4G7118 (2)
C2G1—C3G1—C4G1—C5G134 (2)C1G6—C2G6—C3G6—C4G644.5 (15)
C2G1—C3G1—C4G1—O4G1157.1 (18)C1G6—C2G6—C3G6—O3G6166.4 (12)
O3G1—C3G1—C4G1—C5G1163.0 (15)O2G6—C2G6—C3G6—C4G6172.5 (15)
O3G1—C3G1—C4G1—O4G174 (2)O2G6—C2G6—C3G6—O3G665.6 (17)
C3G1—C4G1—C5G1—O5G151.8 (18)C2G6—C3G6—C4G6—C5G637.2 (19)
C3G1—C4G1—C5G1—C6G1150 (2)C2G6—C3G6—C4G6—O4G6148 (2)
O4G1—C4G1—C5G1—O5G1170.1 (16)O3G6—C3G6—C4G6—C5G6162.4 (14)
O4G1—C4G1—C5G1—C6G192 (3)O3G6—C3G6—C4G6—O4G623 (3)
C3G1—C4G1—O4G1—C1G7126 (2)C3G6—C4G6—C5G6—O5G642 (2)
C5G1—C4G1—O4G1—C1G7110 (2)C3G6—C4G6—C5G6—C6G6169 (2)
C4G1—C5G1—O5G1—C1G166 (2)O4G6—C4G6—C5G6—O5G6142 (2)
C6G1—C5G1—O5G1—C1G1171 (2)O4G6—C4G6—C5G6—C6G615 (3)
C4G1—C5G1—C6G1—O6G1152 (3)C3G6—C4G6—O4G6—C1G5156 (6)
O5G1—C5G1—C6G1—O6G196 (4)C5G6—C4G6—O4G6—C1G519 (8)
C4G1—O4G1—C1G7—C2G7126 (2)C4G6—C5G6—O5G6—C1G655 (2)
C4G1—O4G1—C1G7—O5G7122 (2)C6G6—C5G6—O5G6—C1G6173 (2)
O5G2—C1G2—C2G2—C3G257 (2)C4G6—C5G6—C6G6—O6G634 (4)
O5G2—C1G2—C2G2—O2G2172 (2)O5G6—C5G6—C6G6—O6G696 (3)
O4G3—C1G2—C2G2—C3G265 (2)O4G1—C1G7—C2G7—C3G754 (2)
O4G3—C1G2—C2G2—O2G266 (2)O4G1—C1G7—C2G7—O2G774 (2)
C2G2—C1G2—O5G2—C5G268 (2)O5G7—C1G7—C2G7—C3G756.7 (17)
O4G3—C1G2—O5G2—C5G240 (3)O5G7—C1G7—C2G7—O2G7175.4 (14)
C2G2—C1G2—O4G3—C4G3113 (2)O4G1—C1G7—O5G7—C5G731 (3)
O5G2—C1G2—O4G3—C4G3132 (2)C2G7—C1G7—O5G7—C5G769 (2)
C1G2—C2G2—C3G2—C4G228 (2)C1G7—C2G7—C3G7—C4G732 (2)
C1G2—C2G2—C3G2—O3G2153.3 (17)C1G7—C2G7—C3G7—O3G7165.0 (15)
O2G2—C2G2—C3G2—C4G2159.5 (16)O2G7—C2G7—C3G7—C4G7159.8 (18)
O2G2—C2G2—C3G2—O3G275 (2)O2G7—C2G7—C3G7—O3G767 (2)
C2G2—C3G2—C4G2—C5G211 (2)C2G7—C3G7—C4G7—C5G719 (2)
C2G2—C3G2—C4G2—O4G2171 (2)C2G7—C3G7—C4G7—O4G7116.6 (19)
O3G2—C3G2—C4G2—C5G2136 (2)O3G7—C3G7—C4G7—C5G7152.6 (15)
O3G2—C3G2—C4G2—O4G263 (3)O3G7—C3G7—C4G7—O4G7109 (2)
C3G2—C4G2—C5G2—O5G220 (2)C3G7—C4G7—C5G7—O5G729 (2)
C3G2—C4G2—C5G2—C6G2136 (3)C3G7—C4G7—C5G7—C6G7126 (2)
O4G2—C4G2—C5G2—O5G2180 (2)O4G7—C4G7—C5G7—O5G7151 (2)
O4G2—C4G2—C5G2—C6G264 (4)O4G7—C4G7—C5G7—C6G74 (2)
C3G2—C4G2—O4G2—C1G1157 (5)C3G7—C4G7—O4G7—C1G6118 (2)
C5G2—C4G2—O4G2—C1G143 (6)C5G7—C4G7—O4G7—C1G6126 (2)
C4G2—C5G2—O5G2—C1G250 (2)C4G7—C5G7—O5G7—C1G755 (3)
C6G2—C5G2—O5G2—C1G2178 (2)C6G7—C5G7—O5G7—C1G797 (3)
C4G2—C5G2—C6G2—O6G2132 (3)C4G7—C5G7—C6G7—O6G7105 (3)
O5G2—C5G2—C6G2—O6G2103 (4)O5G7—C5G7—C6G7—O6G7102 (3)
O5G3—C1G3—C2G3—C3G361.7 (19)H33—O2—C10—O188 (5)
O5G3—C1G3—C2G3—O2G3172.5 (16)H33—O2—C10—C999 (3)
O4G4—C1G3—C2G3—C3G3138 (2)C11—N3—C4—C548 (8)
O4G4—C1G3—C2G3—O2G312 (3)C11—N3—C4—C9134 (6)
C2G3—C1G3—O5G3—C5G364 (2)H19—N3—C4—C5123 (4)
O4G4—C1G3—O5G3—C5G3130 (2)H19—N3—C4—C956 (5)
C2G3—C1G3—O4G4—C4G4145 (3)C4—N3—C11—C1257 (7)
O5G3—C1G3—O4G4—C4G415 (4)C4—N3—C11—C16116 (6)
C1G3—C2G3—C3G3—C4G349.2 (17)H19—N3—C11—C12133 (3)
C1G3—C2G3—C3G3—O3G3179.5 (16)H19—N3—C11—C1654 (5)
O2G3—C2G3—C3G3—C4G3174.0 (12)N3—C4—C5—C6160 (4)
O2G3—C2G3—C3G3—O3G354.7 (19)N3—C4—C5—H296 (6)
C2G3—C3G3—C4G3—C5G338.8 (19)C9—C4—C5—C621 (5)
C2G3—C3G3—C4G3—O4G3154.8 (16)C9—C4—C5—H29175 (3)
O3G3—C3G3—C4G3—C5G3170.5 (16)N3—C4—C9—C8169 (3)
O3G3—C3G3—C4G3—O4G374 (2)N3—C4—C9—C102 (6)
C3G3—C4G3—C5G3—O5G340 (2)C5—C4—C9—C812 (5)
C3G3—C4G3—C5G3—C6G3122.5 (19)C5—C4—C9—C10176 (3)
O4G3—C4G3—C5G3—O5G3158 (2)C4—C5—C6—C716 (6)
O4G3—C4G3—C5G3—C6G3119 (2)C4—C5—C6—H30173 (4)
C3G3—C4G3—O4G3—C1G2149.2 (17)H29—C5—C6—C7170 (3)
C5G3—C4G3—O4G3—C1G289 (2)H29—C5—C6—H3019 (7)
C4G3—C5G3—O5G3—C1G353 (2)C5—C6—C7—C80 (4)
C6G3—C5G3—O5G3—C1G3143 (2)C5—C6—C7—H31163 (4)
C4G3—C5G3—C6G3—O6G373 (3)H30—C6—C7—C8174 (3)
O5G3—C5G3—C6G3—O6G3172 (3)H30—C6—C7—H3111 (6)
O5G4—C1G4—C2G4—C3G457 (2)C6—C7—C8—C95 (5)
O5G4—C1G4—C2G4—O2G4173.6 (18)C6—C7—C8—H32165 (3)
O4G5—C1G4—C2G4—C3G4110 (2)H31—C7—C8—C9172 (3)
O4G5—C1G4—C2G4—O2G419 (3)H31—C7—C8—H3229 (5)
C2G4—C1G4—O5G4—C5G464 (2)C7—C8—C9—C42 (5)
O4G5—C1G4—O5G4—C5G498 (3)C7—C8—C9—C10173 (3)
C2G4—C1G4—O4G5—C4G5163 (5)H32—C8—C9—C4160 (3)
O5G4—C1G4—O4G5—C4G534 (7)H32—C8—C9—C1011 (4)
C1G4—C2G4—C3G4—C4G444 (2)C4—C9—C10—O115 (6)
C1G4—C2G4—C3G4—O3G4172.2 (15)C4—C9—C10—O2172 (3)
O2G4—C2G4—C3G4—C4G4172.4 (17)C8—C9—C10—O1173 (4)
O2G4—C2G4—C3G4—O3G460 (2)C8—C9—C10—O20 (4)
C2G4—C3G4—C4G4—C5G437 (2)N3—C11—C12—C13176 (3)
C2G4—C3G4—C4G4—O4G4160.4 (19)N3—C11—C12—H206 (4)
O3G4—C3G4—C4G4—C5G4165.8 (15)C16—C11—C12—C132 (4)
O3G4—C3G4—C4G4—O4G471.0 (18)C16—C11—C12—H20179 (3)
C3G4—C4G4—C5G4—O5G443 (2)N3—C11—C16—C15179 (3)
C3G4—C4G4—C5G4—C6G4142 (2)N3—C11—C16—C1711 (5)
O4G4—C4G4—C5G4—O5G4139 (2)C12—C11—C16—C157 (4)
O4G4—C4G4—C5G4—C6G4122 (3)C12—C11—C16—C17177 (3)
C3G4—C4G4—O4G4—C1G3172 (3)C11—C12—C13—C144 (4)
C5G4—C4G4—O4G4—C1G374 (4)C11—C12—C13—H21170 (3)
C4G4—C5G4—O5G4—C1G457 (2)H20—C12—C13—C14173 (3)
C6G4—C5G4—O5G4—C1G4164 (2)H20—C12—C13—H217 (5)
C4G4—C5G4—C6G4—O6G4110 (3)C12—C13—C14—C156 (5)
O5G4—C5G4—C6G4—O6G4135 (3)C12—C13—C14—H22176 (3)
O5G5—C1G5—C2G5—C3G553.4 (17)H21—C13—C14—C15172 (3)
O5G5—C1G5—C2G5—O2G5173.8 (14)H21—C13—C14—H2218 (5)
O4G6—C1G5—C2G5—C3G595 (2)C13—C14—C15—C162 (5)
O4G6—C1G5—C2G5—O2G538 (2)C13—C14—C15—C18173 (3)
C2G5—C1G5—O5G5—C5G561.8 (18)H22—C14—C15—C16171 (3)
O4G6—C1G5—O5G5—C5G587 (2)H22—C14—C15—C184 (4)
C2G5—C1G5—O4G6—C4G6167 (7)C14—C15—C16—C115 (4)
O5G5—C1G5—O4G6—C4G622 (9)C14—C15—C16—C17176 (2)
C1G5—C2G5—C3G5—C4G543.3 (18)C18—C15—C16—C11179 (2)
C1G5—C2G5—C3G5—O3G5169.6 (13)C18—C15—C16—C1710 (4)
O2G5—C2G5—C3G5—C4G5175.0 (16)C14—C15—C18—H23131 (2)
O2G5—C2G5—C3G5—O3G559 (2)C14—C15—C18—H24116 (3)
C2G5—C3G5—C4G5—C5G541.5 (18)C14—C15—C18—H254 (3)
C2G5—C3G5—C4G5—O4G5179.9 (18)C16—C15—C18—H2356 (3)
O3G5—C3G5—C4G5—C5G5167.3 (14)C16—C15—C18—H2458 (3)
O3G5—C3G5—C4G5—O4G554 (2)C16—C15—C18—H25178 (2)
C3G5—C4G5—C5G5—O5G551 (2)C11—C16—C17—H26128 (3)
C3G5—C4G5—C5G5—C6G5166 (3)C11—C16—C17—H2715 (3)
O4G5—C4G5—C5G5—O5G5174 (2)C11—C16—C17—H2892 (3)
O4G5—C4G5—C5G5—C6G531 (4)C15—C16—C17—H2643 (3)
C3G5—C4G5—O4G5—C1G4162 (5)C15—C16—C17—H27156 (2)
C5G5—C4G5—O4G5—C1G462 (6)C15—C16—C17—H2897 (3)
(2) β-cyclodextrin/mefenamic acid inclusion complex top
Crystal data top
C55.5H13.5N.9O36.8V = 3637.7 (2) Å3
Mr = 1281.59Z = 2
Monoclinic, P_1_21_1Dx = 1.17 Mg m3
Hall symbol: p_2ybSynchrotron radiation, λ = 0.800807 Å
a = 15.4797 (5) ÅT = 295 K
b = 25.5892 (10) Åwhite
c = 9.2973 (4) Åcylinder, ? × 1 mm
β = 98.976 (3)°
Data collection top
ESRF BM16
diffractometer
Data collection mode: transmission
Si(111) double monochromatorScan method: continuous
Specimen mounting: packed powder pellet2θmin = 3.205°, 2θmax = 39.995°, 2θstep = 0.005°
Refinement top
Rp = 0.1127359 data points
Rwp = 0.157141 parameters
Rexp = 0.024126 restraints
χ2 = 50.126(Δ/σ)max = 0.24
Crystal data top
C55.5H13.5N.9O36.8β = 98.976 (3)°
Mr = 1281.59V = 3637.7 (2) Å3
Monoclinic, P_1_21_1Z = 2
a = 15.4797 (5) ÅSynchrotron radiation, λ = 0.800807 Å
b = 25.5892 (10) ÅT = 295 K
c = 9.2973 (4) Åcylinder, ? × 1 mm
Data collection top
ESRF BM16
diffractometer
Scan method: continuous
Specimen mounting: packed powder pellet2θmin = 3.205°, 2θmax = 39.995°, 2θstep = 0.005°
Data collection mode: transmission
Refinement top
Rp = 0.1127359 data points
Rwp = 0.157141 parameters
Rexp = 0.024126 restraints
χ2 = 50.126(Δ/σ)max = 0.24
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1G10.0863 (13)0.7829 (9)0.009 (3)0.05794*
C2G10.1279 (12)0.7796 (9)0.133 (3)0.05794*
C3G10.2253 (12)0.7678 (8)0.111 (3)0.05794*
C4G10.2763 (12)0.7879 (8)0.031 (3)0.05794*
C5G10.2238 (17)0.7859 (8)0.159 (3)0.05794*
O2G10.0793 (14)0.7495 (9)0.246 (3)0.05131*
O3G10.2642 (15)0.7837 (9)0.233 (3)0.05131*
O5G10.1406 (17)0.8108 (8)0.121 (3)0.05131*
O6G10.258 (4)0.8674 (16)0.302 (5)0.05131*
C6G10.231 (5)0.814 (2)0.308 (4)0.05794*
O4G10.3546 (15)0.7782 (15)0.021 (3)0.05131*
C1G20.1051 (18)0.6759 (10)0.289 (2)0.05794*
C2G20.1817 (14)0.6892 (10)0.167 (3)0.05794*
C3G20.1529 (15)0.7113 (9)0.030 (3)0.05794*
C4G20.0658 (16)0.7404 (9)0.056 (3)0.05794*
C5G20.0079 (14)0.7371 (9)0.207 (3)0.05794*
O2G20.2441 (13)0.6483 (10)0.136 (4)0.05131*
O3G20.2192 (18)0.7438 (10)0.047 (3)0.05131*
O5G20.0532 (19)0.7218 (10)0.324 (3)0.05131*
O6G20.115 (3)0.7882 (19)0.293 (6)0.05131*
C6G20.032 (3)0.7736 (19)0.329 (5)0.05794*
O4G20.0237 (18)0.7457 (13)0.040 (5)0.05131*
C1G30.0612 (11)0.5010 (10)0.417 (2)0.05794*
C2G30.1516 (10)0.4909 (10)0.3243 (19)0.05794*
C3G30.1818 (13)0.5403 (10)0.240 (2)0.05794*
C4G30.1746 (12)0.5894 (10)0.334 (2)0.05794*
C5G30.0919 (12)0.5908 (10)0.450 (2)0.05794*
O2G30.1500 (10)0.4462 (10)0.2336 (18)0.05131*
O3G30.2643 (17)0.5354 (11)0.150 (3)0.05131*
O5G30.0674 (15)0.5419 (10)0.520 (2)0.05131*
O6G30.047 (3)0.587 (2)0.716 (4)0.05131*
C6G30.121 (2)0.5931 (15)0.602 (3)0.05794*
O4G30.1029 (16)0.6189 (11)0.292 (5)0.05131*
C1G40.2368 (12)0.4421 (11)0.741 (3)0.05794*
C2G40.1779 (12)0.3957 (10)0.681 (2)0.05794*
C3G40.0941 (13)0.4140 (9)0.5873 (19)0.05794*
C4G40.0515 (14)0.4600 (10)0.654 (3)0.05794*
C5G40.1157 (14)0.4997 (10)0.733 (2)0.05794*
O2G40.2240 (11)0.3577 (11)0.612 (3)0.05131*
O3G40.0335 (11)0.3726 (10)0.547 (2)0.05131*
O5G40.1889 (13)0.4762 (10)0.8221 (19)0.05131*
O6G40.0094 (19)0.5406 (19)0.896 (5)0.05131*
C6G40.082 (3)0.5059 (15)0.883 (3)0.05794*
O4G40.017 (2)0.4695 (12)0.534 (3)0.05131*
C1G50.5555 (14)0.5057 (11)0.583 (3)0.05794*
C2G50.5382 (11)0.4475 (10)0.610 (3)0.05794*
C3G50.4417 (11)0.4332 (10)0.585 (2)0.05794*
C4G50.3862 (12)0.4740 (11)0.648 (3)0.05794*
C5G50.4146 (13)0.5301 (10)0.622 (3)0.05794*
O2G50.5927 (11)0.4136 (12)0.544 (4)0.05131*
O3G50.4279 (14)0.3820 (10)0.636 (2)0.05131*
O5G50.5061 (13)0.5382 (10)0.665 (3)0.05131*
O6G50.3548 (12)0.6286 (13)0.667 (2)0.05131*
C6G50.3653 (17)0.5741 (14)0.704 (2)0.05794*
O4G50.304 (2)0.4415 (14)0.640 (4)0.05131*
C1G60.6048 (9)0.6559 (9)0.320 (3)0.05794*
C2G60.5745 (11)0.6151 (9)0.200 (2)0.05794*
C3G60.5487 (9)0.5634 (9)0.263 (2)0.05794*
C4G60.6133 (11)0.5455 (10)0.394 (3)0.05794*
C5G60.6527 (15)0.5897 (11)0.496 (3)0.05794*
O2G60.5094 (15)0.6356 (10)0.089 (3)0.05131*
O3G60.5343 (10)0.5231 (9)0.156 (2)0.05131*
O5G60.6760 (11)0.6352 (10)0.421 (3)0.05131*
O6G60.648 (3)0.6331 (19)0.737 (5)0.05131*
C6G60.614 (4)0.591 (2)0.641 (5)0.05794*
O4G60.5369 (14)0.5348 (15)0.451 (3)0.05131*
C1G70.4190 (13)0.8009 (8)0.080 (3)0.05794*
C2G70.4749 (12)0.7878 (9)0.040 (2)0.05794*
C3G70.5274 (11)0.7376 (9)0.006 (2)0.05794*
C4G70.5576 (13)0.7253 (9)0.154 (3)0.05794*
C5G70.5090 (18)0.7542 (9)0.263 (2)0.05794*
O2G70.4248 (15)0.7875 (9)0.183 (2)0.05131*
O3G70.5954 (13)0.7304 (9)0.091 (3)0.05131*
O5G70.4747 (17)0.8045 (9)0.218 (2)0.05131*
O6G70.435 (3)0.7441 (19)0.474 (5)0.05131*
C6G70.4207 (18)0.750 (3)0.321 (4)0.05794*
O4G70.6084 (13)0.6800 (10)0.184 (3)0.05131*
O10.157 (2)0.579 (2)0.092 (5)0.05131*.90000
O20.275 (3)0.615 (2)0.134 (2)0.05131*.90000
N30.282 (2)0.5182 (14)0.083 (3)0.05131*.90000
C40.274 (3)0.5501 (12)0.203 (3)0.05794*.90000
C50.284 (3)0.5553 (8)0.354 (4)0.05794*.90000
C60.257 (3)0.6014 (14)0.4155 (14)0.05794*.90000
C70.238 (3)0.6460 (9)0.327 (3)0.05794*.90000
C80.227 (3)0.6403 (9)0.175 (3)0.05794*.90000
C90.259 (2)0.5946 (12)0.116 (3)0.05794*.90000
C100.2337 (18)0.590 (2)0.045 (3)0.05794*.90000
C110.3303 (17)0.4712 (11)0.110 (4)0.05794*.90000
C120.4131 (17)0.4834 (10)0.071 (4)0.05794*.90000
C130.4840 (11)0.4492 (12)0.102 (4)0.05794*.90000
C140.4713 (14)0.4035 (10)0.184 (4)0.05794*.90000
C150.3891 (13)0.3904 (10)0.223 (4)0.05794*.90000
C160.3148 (14)0.4233 (10)0.178 (4)0.05794*.90000
C170.2285 (16)0.4139 (5)0.2259 (19)0.05794*.90000
C180.3801 (7)0.3390 (7)0.2957 (15)0.05794*.90000
H190.248180.513280.017630.07000*.90000
H200.435750.512810.018460.07000*.90000
H210.545370.450140.079310.07000*.90000
H220.517170.376390.210260.07000*.90000
H230.326380.319380.245080.07000*.90000
H240.364730.349730.391730.07000*.90000
H250.436340.318410.307770.07000*.90000
H260.216990.379120.184400.07000*.90000
H270.196650.434600.144300.07000*.90000
H280.231740.426520.306740.07000*.90000
H290.297570.520310.400320.07000*.90000
H300.261290.596140.523560.07000*.90000
H310.220230.675970.384750.07000*.90000
H320.204390.672890.122400.07000*.90000
H330.250440.612900.235200.07000*.90000
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
Geometric parameters (Å, º) top
C1G1—O4G21.42 (4)C5G5—C6G51.62 (4)
C1G1—O5G11.43 (3)O6G5—C6G51.44 (5)
C1G1—C2G11.56 (4)C1G6—O4G71.41 (3)
C2G1—O2G11.42 (3)C1G6—O5G61.43 (3)
C2G1—C3G11.52 (3)C1G6—C2G61.55 (3)
C3G1—O3G11.42 (4)C2G6—O2G61.42 (3)
C3G1—C4G11.52 (3)C2G6—C3G61.53 (3)
C4G1—O4G11.40 (3)C3G6—O3G61.42 (3)
C4G1—C5G11.54 (4)C3G6—C4G61.52 (3)
C5G1—O5G11.43 (3)C4G6—O4G61.40 (3)
C5G1—C6G11.56 (5)C4G6—C5G61.54 (4)
O6G1—C6G11.43 (7)C5G6—O5G61.43 (4)
O4G1—C1G71.39 (3)C5G6—C6G61.56 (6)
C1G2—O5G21.43 (4)O6G6—C6G61.44 (7)
C1G2—O4G31.46 (4)C1G7—O5G71.43 (3)
C1G2—C2G21.55 (3)C1G7—C2G71.55 (3)
C2G2—O2G21.42 (3)C2G7—O2G71.43 (3)
C2G2—C3G21.52 (4)C2G7—C3G71.53 (3)
C3G2—O3G21.42 (3)C3G7—O3G71.42 (3)
C3G2—C4G21.53 (3)C3G7—C4G71.53 (3)
C4G2—O4G21.42 (4)C4G7—O4G71.40 (3)
C4G2—C5G21.54 (4)C4G7—C5G71.54 (3)
C5G2—O5G21.44 (4)C5G7—O5G71.43 (3)
C5G2—C6G21.52 (5)C5G7—C6G71.55 (4)
O6G2—C6G21.43 (6)O6G7—C6G71.41 (6)
C1G3—O5G31.44 (3)O1—C101.24 (4)
C1G3—O4G41.44 (4)O2—H330.96 (2)
C1G3—C2G31.54 (2)O2—C101.29 (5)
C2G3—O2G31.42 (3)N3—H191.01 (3)
C2G3—C3G31.52 (3)N3—C41.40 (4)
C3G3—O3G31.42 (3)N3—C111.41 (5)
C3G3—C4G31.53 (3)C4—C51.39 (5)
C4G3—O4G31.45 (4)C4—C91.40 (4)
C4G3—C5G31.54 (3)C5—H291.00 (2)
C5G3—O5G31.43 (3)C5—C61.40 (4)
C5G3—C6G31.55 (4)C6—H301.006 (14)
C5G3—O4G31.62 (5)C6—C71.41 (4)
O6G3—C6G31.44 (5)C7—H311.00 (3)
C1G4—O5G41.43 (3)C7—C81.40 (4)
C1G4—O4G51.51 (4)C8—H321.00 (3)
C1G4—C2G41.55 (3)C8—C91.41 (4)
C2G4—O2G41.42 (4)C9—C101.49 (4)
C2G4—C3G41.52 (3)C11—C161.42 (4)
C3G4—O3G41.43 (3)C11—C121.42 (4)
C3G4—C4G41.53 (3)C12—H200.99 (3)
C4G4—O4G41.43 (4)C12—C131.40 (3)
C4G4—C5G41.53 (3)C13—H211.01 (2)
C5G4—O5G41.43 (3)C13—C141.43 (4)
C5G4—C6G41.58 (4)C14—H221.00 (2)
O6G4—C6G41.45 (6)C14—C151.42 (4)
C1G5—O4G61.42 (4)C15—C161.43 (3)
C1G5—O5G51.43 (4)C15—C181.50 (3)
C1G5—C2G51.54 (4)C16—C171.49 (4)
C2G5—O2G51.42 (4)C17—H280.812 (17)
C2G5—C3G51.52 (2)C17—H260.975 (14)
C3G5—O3G51.42 (4)C17—H270.991 (17)
C3G5—C4G51.53 (3)C18—H240.998 (14)
C4G5—O4G51.51 (4)C18—H251.009 (13)
C4G5—C5G51.53 (4)C18—H231.021 (13)
C5G5—O5G51.43 (3)
O4G2—C1G1—O5G1122 (3)O6G5—C6G5—C5G5127 (2)
O4G2—C1G1—C2G1122 (3)C1G4—O4G5—C4G5128 (3)
O5G1—C1G1—C2G1112 (2)O4G7—C1G6—O5G6127.7 (17)
O2G1—C2G1—C3G1113 (2)O4G7—C1G6—C2G672.5 (17)
O2G1—C2G1—C1G1114.5 (19)O5G6—C1G6—C2G6109.8 (19)
C3G1—C2G1—C1G1115.4 (19)O2G6—C2G6—C3G6113.5 (17)
O3G1—C3G1—C2G1112 (2)O2G6—C2G6—C1G6112 (2)
O3G1—C3G1—C4G1111.7 (18)C3G6—C2G6—C1G6112.0 (18)
C2G1—C3G1—C4G1115 (2)O3G6—C3G6—C4G6110.5 (19)
O4G1—C4G1—C3G190 (2)O3G6—C3G6—C2G6112.6 (18)
O4G1—C4G1—C5G1149 (2)C4G6—C3G6—C2G6113.0 (15)
C3G1—C4G1—C5G1113.2 (17)O4G6—C4G6—C3G682.8 (16)
O5G1—C5G1—C4G1111 (2)O4G6—C4G6—C5G6101 (2)
O5G1—C5G1—C6G187 (3)C3G6—C4G6—C5G6115 (2)
C4G1—C5G1—C6G1134 (3)O5G6—C5G6—C4G6114 (2)
C1G1—O5G1—C5G1111 (2)O5G6—C5G6—C6G6124 (3)
O6G1—C6G1—C5G1113 (4)C4G6—C5G6—C6G6112 (3)
C1G7—O4G1—C4G1105 (2)C5G6—O5G6—C1G6113.1 (17)
O5G2—C1G2—O4G3144 (2)O6G6—C6G6—C5G6114 (4)
O5G2—C1G2—C2G2109 (2)C4G6—O4G6—C1G5111 (2)
O4G3—C1G2—C2G2104 (2)O4G1—C1G7—O5G7154 (2)
O2G2—C2G2—C3G2113 (2)O4G1—C1G7—C2G781.1 (18)
O2G2—C2G2—C1G2114 (2)O5G7—C1G7—C2G7109.4 (18)
C3G2—C2G2—C1G2114 (2)O2G7—C2G7—C3G7112.5 (19)
O3G2—C3G2—C2G2111 (2)O2G7—C2G7—C1G7112.6 (17)
O3G2—C3G2—C4G2110 (2)C3G7—C2G7—C1G7111.9 (17)
C2G2—C3G2—C4G2114.6 (19)O3G7—C3G7—C2G7114 (2)
O4G2—C4G2—C3G2152 (3)O3G7—C3G7—C4G7112.1 (17)
O4G2—C4G2—C5G270 (2)C2G7—C3G7—C4G7116.6 (19)
C3G2—C4G2—C5G2119 (2)O4G7—C4G7—C3G7116 (2)
O5G2—C5G2—C6G278 (3)O4G7—C4G7—C5G7126 (2)
O5G2—C5G2—C4G2115 (2)C3G7—C4G7—C5G7116.0 (17)
C6G2—C5G2—C4G2139 (3)O5G7—C5G7—C4G7116 (2)
C1G2—O5G2—C5G2112 (2)O5G7—C5G7—C6G782 (3)
O6G2—C6G2—C5G2105 (4)C4G7—C5G7—C6G7138 (3)
C1G1—O4G2—C4G2142 (3)C5G7—O5G7—C1G7110.6 (19)
O5G3—C1G3—O4G488.6 (19)O6G7—C6G7—C5G7110 (3)
O5G3—C1G3—C2G3110.2 (17)C4G7—O4G7—C1G6116 (2)
O4G4—C1G3—C2G3128 (2)H33—O2—C10116 (4)
O2G3—C2G3—C3G3113.2 (16)H19—N3—C4135 (4)
O2G3—C2G3—C1G3111.4 (16)H19—N3—C11104 (3)
C3G3—C2G3—C1G3109.0 (19)C4—N3—C11118 (3)
O3G3—C3G3—C2G3114 (2)C5—C4—C9119 (3)
O3G3—C3G3—C4G3113 (2)C5—C4—N3148 (3)
C2G3—C3G3—C4G3113.4 (16)C9—C4—N392 (3)
O4G3—C4G3—C3G3105 (2)H29—C5—C4109 (2)
O4G3—C4G3—C5G366 (2)H29—C5—C6129 (3)
C3G3—C4G3—C5G3113.5 (18)C4—C5—C6120 (2)
O5G3—C5G3—C4G3115 (2)H30—C6—C5109 (3)
O5G3—C5G3—C6G373 (2)H30—C6—C7132 (3)
O5G3—C5G3—O4G3141 (2)C5—C6—C7119 (2)
C4G3—C5G3—C6G3108.0 (18)H31—C7—C8129 (3)
C4G3—C5G3—O4G354.4 (14)H31—C7—C6111 (3)
C6G3—C5G3—O4G3144 (2)C8—C7—C6119 (2)
C5G3—O5G3—C1G3111.8 (19)H32—C8—C7112 (2)
O6G3—C6G3—C5G3111 (3)H32—C8—C9128 (3)
C4G3—O4G3—C1G2121 (3)C7—C8—C9119 (2)
C4G3—O4G3—C5G359.9 (18)C4—C9—C8119 (3)
C1G2—O4G3—C5G3117 (3)C4—C9—C10121 (3)
O5G4—C1G4—O4G5143 (3)C8—C9—C10114 (3)
O5G4—C1G4—C2G4109.4 (17)O1—C10—O2116 (3)
O4G5—C1G4—C2G4101 (2)O1—C10—C9118 (3)
O2G4—C2G4—C3G4113.4 (18)O2—C10—C9122 (3)
O2G4—C2G4—C1G4112.2 (17)N3—C11—C16134 (3)
C3G4—C2G4—C1G4112 (2)N3—C11—C12104 (3)
O3G4—C3G4—C2G4113 (2)C16—C11—C12122 (2)
O3G4—C3G4—C4G4111.8 (18)H20—C12—C13104 (3)
C2G4—C3G4—C4G4113.0 (17)H20—C12—C11134 (3)
O4G4—C4G4—C3G498 (2)C13—C12—C11121 (3)
O4G4—C4G4—C5G4128 (2)H21—C13—C12133 (3)
C3G4—C4G4—C5G4114.7 (18)H21—C13—C14110 (2)
O5G4—C5G4—C4G4113 (2)C12—C13—C14117 (2)
O5G4—C5G4—C6G482.8 (19)H22—C14—C15114 (3)
C4G4—C5G4—C6G4102 (2)H22—C14—C13123 (2)
C5G4—O5G4—C1G4112.3 (17)C15—C14—C13122 (2)
O6G4—C6G4—C5G4120 (3)C14—C15—C16120 (3)
C4G4—O4G4—C1G3153 (3)C14—C15—C18118.3 (19)
O4G6—C1G5—O5G596 (2)C16—C15—C18121 (2)
O4G6—C1G5—C2G5129 (2)C11—C16—C15117 (2)
O5G5—C1G5—C2G5111 (2)C11—C16—C17120 (2)
O2G5—C2G5—C3G5115 (2)C15—C16—C17122 (3)
O2G5—C2G5—C1G5113 (2)H28—C17—H26135 (2)
C3G5—C2G5—C1G5113.5 (18)H28—C17—H27116.6 (18)
O3G5—C3G5—C2G5111.4 (18)H28—C17—C16106 (2)
O3G5—C3G5—C4G5112 (2)H26—C17—H2798.4 (15)
C2G5—C3G5—C4G5112 (2)H26—C17—C1698 (2)
O4G5—C4G5—C3G597 (2)H27—C17—C1692.7 (19)
O4G5—C4G5—C5G5140 (2)H24—C18—H25111.5 (12)
C3G5—C4G5—C5G5113 (2)H24—C18—H23104.9 (11)
O5G5—C5G5—C4G5113 (2)H24—C18—C15102.4 (19)
O5G5—C5G5—C6G5107 (2)H25—C18—H23114.9 (17)
C4G5—C5G5—C6G5114 (2)H25—C18—C15111.7 (14)
C5G5—O5G5—C1G5111 (2)H23—C18—C15110.5 (14)
O5G1—C1G1—C2G1—C3G142 (3)O3G5—C3G5—C4G5—O4G540 (2)
O5G1—C1G1—C2G1—O2G1176 (2)C3G5—C4G5—C5G5—O5G551 (3)
O4G2—C1G1—C2G1—C3G1114 (2)C3G5—C4G5—C5G5—C6G5173.0 (18)
O4G2—C1G1—C2G1—O2G120 (3)O4G5—C4G5—C5G5—O5G5174 (3)
C2G1—C1G1—O5G1—C5G160 (3)O4G5—C4G5—C5G5—C6G552 (5)
O4G2—C1G1—O5G1—C5G196 (3)C3G5—C4G5—O4G5—C1G4148 (3)
C2G1—C1G1—O4G2—C4G2114 (6)C5G5—C4G5—O4G5—C1G473 (5)
O5G1—C1G1—O4G2—C4G293 (6)C4G5—C5G5—O5G5—C1G562 (3)
C1G1—C2G1—C3G1—C4G130 (3)C6G5—C5G5—O5G5—C1G5172 (2)
C1G1—C2G1—C3G1—O3G1159 (2)C4G5—C5G5—C6G5—O6G5158 (2)
O2G1—C2G1—C3G1—C4G1165 (2)O5G5—C5G5—C6G5—O6G576 (3)
O2G1—C2G1—C3G1—O3G167 (3)O5G6—C1G6—C2G6—C3G657 (2)
C2G1—C3G1—C4G1—C5G135 (2)O5G6—C1G6—C2G6—O2G6174 (2)
C2G1—C3G1—C4G1—O4G1167 (2)O4G7—C1G6—C2G6—C3G6178.6 (16)
O3G1—C3G1—C4G1—C5G1163.1 (18)O4G7—C1G6—C2G6—O2G650 (2)
O3G1—C3G1—C4G1—O4G139 (2)C2G6—C1G6—O5G6—C5G662 (3)
C3G1—C4G1—C5G1—O5G152 (2)O4G7—C1G6—O5G6—C5G6145 (3)
C3G1—C4G1—C5G1—C6G1159 (4)C2G6—C1G6—O4G7—C4G7122 (2)
O4G1—C4G1—C5G1—O5G1174 (4)O5G6—C1G6—O4G7—C4G7137 (2)
O4G1—C4G1—C5G1—C6G167 (6)C1G6—C2G6—C3G6—C4G644 (2)
C3G1—C4G1—O4G1—C1G7171 (2)C1G6—C2G6—C3G6—O3G6170.5 (13)
C5G1—C4G1—O4G1—C1G751 (5)O2G6—C2G6—C3G6—C4G6172 (2)
C4G1—C5G1—O5G1—C1G166 (3)O2G6—C2G6—C3G6—O3G661 (2)
C6G1—C5G1—O5G1—C1G1157 (3)C2G6—C3G6—C4G6—C5G637 (3)
C4G1—C5G1—C6G1—O6G137 (7)C2G6—C3G6—C4G6—O4G6136 (2)
O5G1—C5G1—C6G1—O6G180 (5)O3G6—C3G6—C4G6—C5G6164.2 (18)
C4G1—O4G1—C1G7—C2G7171 (3)O3G6—C3G6—C4G6—O4G697 (2)
C4G1—O4G1—C1G7—O5G772 (6)C3G6—C4G6—C5G6—O5G642 (3)
O5G2—C1G2—C2G2—C3G257 (3)C3G6—C4G6—C5G6—C6G6106 (3)
O5G2—C1G2—C2G2—O2G2172 (2)O4G6—C4G6—C5G6—O5G6129 (2)
O4G3—C1G2—C2G2—C3G2108 (3)O4G6—C4G6—C5G6—C6G619 (3)
O4G3—C1G2—C2G2—O2G222 (3)C3G6—C4G6—O4G6—C1G5170 (3)
C2G2—C1G2—O5G2—C5G268 (3)C5G6—C4G6—O4G6—C1G576 (3)
O4G3—C1G2—O5G2—C5G287 (5)C4G6—C5G6—O5G6—C1G655 (3)
C2G2—C1G2—O4G3—C4G366 (4)C6G6—C5G6—O5G6—C1G688 (4)
C2G2—C1G2—O4G3—C5G3135 (2)C4G6—C5G6—C6G6—O6G6178 (3)
O5G2—C1G2—O4G3—C4G3139 (3)O5G6—C5G6—C6G6—O6G634 (5)
O5G2—C1G2—O4G3—C5G369 (5)O4G1—C1G7—C2G7—C3G799 (2)
C1G2—C2G2—C3G2—C4G228 (3)O4G1—C1G7—C2G7—O2G729 (2)
C1G2—C2G2—C3G2—O3G2153 (2)O5G7—C1G7—C2G7—C3G757 (2)
O2G2—C2G2—C3G2—C4G2159 (2)O5G7—C1G7—C2G7—O2G7176 (2)
O2G2—C2G2—C3G2—O3G275 (3)O4G1—C1G7—O5G7—C5G742 (6)
C2G2—C3G2—C4G2—C5G210 (3)C2G7—C1G7—O5G7—C5G769 (3)
C2G2—C3G2—C4G2—O4G2114 (5)C1G7—C2G7—C3G7—C4G732 (2)
O3G2—C3G2—C4G2—C5G2136 (2)C1G7—C2G7—C3G7—O3G7165.1 (18)
O3G2—C3G2—C4G2—O4G2120 (5)O2G7—C2G7—C3G7—C4G7159.7 (19)
C3G2—C4G2—C5G2—O5G220 (3)O2G7—C2G7—C3G7—O3G767 (2)
C3G2—C4G2—C5G2—C6G2120 (4)C2G7—C3G7—C4G7—C5G719 (3)
O4G2—C4G2—C5G2—O5G2171 (3)C2G7—C3G7—C4G7—O4G7177.9 (18)
O4G2—C4G2—C5G2—C6G289 (4)O3G7—C3G7—C4G7—C5G7153 (2)
C3G2—C4G2—O4G2—C1G1137 (5)O3G7—C3G7—C4G7—O4G744 (3)
C5G2—C4G2—O4G2—C1G1107 (6)C3G7—C4G7—C5G7—O5G729 (3)
C4G2—C5G2—O5G2—C1G250 (3)C3G7—C4G7—C5G7—C6G778 (4)
C6G2—C5G2—O5G2—C1G2172 (3)O4G7—C4G7—C5G7—O5G7169 (2)
C4G2—C5G2—C6G2—O6G290 (5)O4G7—C4G7—C5G7—C6G784 (4)
O5G2—C5G2—C6G2—O6G2156 (4)C3G7—C4G7—O4G7—C1G6153.4 (18)
O5G3—C1G3—C2G3—C3G362 (2)C5G7—C4G7—O4G7—C1G68 (3)
O5G3—C1G3—C2G3—O2G3173 (2)C4G7—C5G7—O5G7—C1G755 (3)
O4G4—C1G3—C2G3—C3G3166 (2)C6G7—C5G7—O5G7—C1G785 (2)
O4G4—C1G3—C2G3—O2G368 (3)C4G7—C5G7—C6G7—O6G7122 (4)
C2G3—C1G3—O5G3—C5G364 (2)O5G7—C5G7—C6G7—O6G7118 (5)
O4G4—C1G3—O5G3—C5G3167 (2)H33—O2—C10—O118 (7)
C2G3—C1G3—O4G4—C4G4170 (5)H33—O2—C10—C9172 (4)
O5G3—C1G3—O4G4—C4G456 (6)C11—N3—C4—C513 (9)
C1G3—C2G3—C3G3—C4G349 (2)C11—N3—C4—C9157 (3)
C1G3—C2G3—C3G3—O3G3180 (2)H19—N3—C4—C5144 (6)
O2G3—C2G3—C3G3—C4G3174.0 (16)H19—N3—C4—C946 (6)
O2G3—C2G3—C3G3—O3G355 (2)C4—N3—C11—C12101 (4)
C2G3—C3G3—C4G3—C5G339 (2)C4—N3—C11—C1670 (5)
C2G3—C3G3—C4G3—O4G3109 (2)H19—N3—C11—C1296 (3)
O3G3—C3G3—C4G3—C5G3171 (2)H19—N3—C11—C1693 (4)
O3G3—C3G3—C4G3—O4G3120 (2)N3—C4—C5—C6176 (6)
C3G3—C4G3—C5G3—O5G340 (3)N3—C4—C5—H298 (9)
C3G3—C4G3—C5G3—C6G3119 (2)C9—C4—C5—C616 (6)
C3G3—C4G3—C5G3—O4G397 (2)C9—C4—C5—H29177 (4)
O4G3—C4G3—C5G3—O5G3136 (2)N3—C4—C9—C8167 (3)
O4G3—C4G3—C5G3—C6G3144 (3)N3—C4—C9—C1017 (4)
O4G3—C4G3—C5G3—O4G30 (2)C5—C4—C9—C819 (6)
C3G3—C4G3—O4G3—C1G2145 (3)C5—C4—C9—C10170 (3)
C3G3—C4G3—O4G3—C5G3109 (2)C4—C5—C6—C713 (6)
C5G3—C4G3—O4G3—C1G2106 (4)C4—C5—C6—H30173 (4)
C5G3—C4G3—O4G3—C5G30.0 (14)H29—C5—C6—C7177 (4)
C4G3—C5G3—O5G3—C1G352 (3)H29—C5—C6—H308 (6)
C6G3—C5G3—O5G3—C1G3155 (2)C5—C6—C7—C814 (6)
O4G3—C5G3—O5G3—C1G312 (4)C5—C6—C7—H31179 (3)
C4G3—C5G3—C6G3—O6G3172 (3)H30—C6—C7—C8173 (4)
O5G3—C5G3—C6G3—O6G360 (3)H30—C6—C7—H316 (7)
O4G3—C5G3—C6G3—O6G3134 (4)C6—C7—C8—C917 (6)
C4G3—C5G3—O4G3—C1G2111 (3)C6—C7—C8—H32171 (4)
C4G3—C5G3—O4G3—C4G30.0 (16)H31—C7—C8—C9179 (4)
O5G3—C5G3—O4G3—C1G2162 (3)H31—C7—C8—H326 (6)
O5G3—C5G3—O4G3—C4G387 (3)C7—C8—C9—C420 (5)
C6G3—C5G3—O4G3—C1G241 (4)C7—C8—C9—C10172 (3)
C6G3—C5G3—O4G3—C4G371 (4)H32—C8—C9—C4169 (4)
O5G4—C1G4—C2G4—C3G457 (2)H32—C8—C9—C1017 (6)
O5G4—C1G4—C2G4—O2G4174 (2)C4—C9—C10—O178 (6)
O4G5—C1G4—C2G4—C3G4102 (2)C4—C9—C10—O2127 (5)
O4G5—C1G4—C2G4—O2G427 (3)C8—C9—C10—O174 (6)
C2G4—C1G4—O5G4—C5G464 (3)C8—C9—C10—O281 (5)
O4G5—C1G4—O5G4—C5G480 (4)N3—C11—C12—C13170 (3)
C2G4—C1G4—O4G5—C4G5174 (3)N3—C11—C12—H2012 (5)
O5G4—C1G4—O4G5—C4G541 (5)C16—C11—C12—C132 (5)
C1G4—C2G4—C3G4—C4G444 (2)C16—C11—C12—H20175 (4)
C1G4—C2G4—C3G4—O3G4172.1 (18)N3—C11—C16—C15162 (3)
O2G4—C2G4—C3G4—C4G4172 (2)N3—C11—C16—C176 (6)
O2G4—C2G4—C3G4—O3G460 (3)C12—C11—C16—C158 (5)
C2G4—C3G4—C4G4—C5G437 (3)C12—C11—C16—C17176 (3)
C2G4—C3G4—C4G4—O4G4174 (2)C11—C12—C13—C145 (5)
O3G4—C3G4—C4G4—C5G4165.6 (19)C11—C12—C13—H21177 (4)
O3G4—C3G4—C4G4—O4G457 (2)H20—C12—C13—C14177 (3)
C3G4—C4G4—C5G4—O5G443 (3)H20—C12—C13—H211 (6)
C3G4—C4G4—C5G4—C6G4130 (2)C12—C13—C14—C155 (5)
O4G4—C4G4—C5G4—O5G4165 (3)C12—C13—C14—H22179 (3)
O4G4—C4G4—C5G4—C6G4107 (3)H21—C13—C14—C15176 (3)
C3G4—C4G4—O4G4—C1G3116 (6)H21—C13—C14—H222 (5)
C5G4—C4G4—O4G4—C1G314 (8)C13—C14—C15—C160 (5)
C4G4—C5G4—O5G4—C1G457 (3)C13—C14—C15—C18174 (3)
C6G4—C5G4—O5G4—C1G4158 (2)H22—C14—C15—C16173 (3)
C4G4—C5G4—C6G4—O6G482 (4)H22—C14—C15—C180 (5)
O5G4—C5G4—C6G4—O6G4165 (4)C14—C15—C16—C117 (5)
O5G5—C1G5—C2G5—C3G553 (3)C14—C15—C16—C17175 (3)
O5G5—C1G5—C2G5—O2G5174 (2)C18—C15—C16—C11180 (3)
O4G6—C1G5—C2G5—C3G563 (3)C18—C15—C16—C1712 (5)
O4G6—C1G5—C2G5—O2G570 (3)C14—C15—C18—H23130 (3)
C2G5—C1G5—O5G5—C5G562 (3)C14—C15—C18—H24119 (3)
O4G6—C1G5—O5G5—C5G574 (3)C14—C15—C18—H250 (3)
C2G5—C1G5—O4G6—C4G6106 (3)C16—C15—C18—H2343 (4)
O5G5—C1G5—O4G6—C4G6131 (3)C16—C15—C18—H2469 (3)
C1G5—C2G5—C3G5—C4G543 (3)C16—C15—C18—H25172 (3)
C1G5—C2G5—C3G5—O3G5170 (2)C11—C16—C17—H26132 (3)
O2G5—C2G5—C3G5—C4G5175 (2)C11—C16—C17—H2733 (3)
O2G5—C2G5—C3G5—O3G558 (3)C11—C16—C17—H2886 (3)
C2G5—C3G5—C4G5—C5G541 (3)C15—C16—C17—H2661 (3)
C2G5—C3G5—C4G5—O4G5166 (2)C15—C16—C17—H27160 (3)
O3G5—C3G5—C4G5—C5G5167.3 (19)C15—C16—C17—H2882 (3)

Experimental details

(1)(2)
Crystal data
Chemical formulaC55.5H13.5N0.9O36.8C55.5H13.5N.9O36.8
Mr1281.591281.59
Crystal system, space groupMonoclinic, P_21Monoclinic, P_1_21_1
Temperature (K)295295
a, b, c (Å)15.4797 (9), 25.5892 (15), 9.2973 (5)15.4797 (5), 25.5892 (10), 9.2973 (4)
β (°) 98.976 (7) 98.976 (3)
V3)3637.7 (4)3637.7 (2)
Z22
Radiation typeSynchrotron, λ = 0.800807 ÅSynchrotron, λ = 0.800807 Å
µ (mm1)??
Specimen shape, size (mm)Cylinder, ? × 1Cylinder, ? × 1
Data collection
DiffractometerESRF BM16
diffractometer
ESRF BM16
diffractometer
Specimen mountingPacked powder pelletPacked powder pellet
Data collection modeTransmissionTransmission
Scan methodContinuousContinuous
2θ values (°)2θmin = 3.205 2θmax = 39.995 2θstep = 0.0052θmin = 3.205 2θmax = 39.995 2θstep = 0.005
Refinement
R factors and goodness of fitRp = 0.098, Rwp = 0.133, Rexp = 0.024, χ2 = 36.966Rp = 0.112, Rwp = 0.157, Rexp = 0.024, χ2 = 50.126
No. of data points73597359
No. of parameters141141
No. of restraints126126
(Δ/σ)max0.320.24

Computer programs: MRIA, GSAS, DIAMOND.

 

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