Supporting Information for. Linker-Directed Vertex Desymmetrization for the Production of Coordination Polymers. with High Porosity
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1 Supporting Information for Linker-Directed Vertex Desymmetrization for the Production of Coordination Polymers with High Porosity Jennifer K. Schnobrich, Olivier Lebel,, Katie A. Cychosz, Anne Dailly, Antek G. Wong-Foy, and Adam J. Matzger*, Department of Chemistry and Macromolecular Science and Engineering Program, The University of Michigan, 93 North University Avenue, Ann Arbor, Michigan, Chemical Sciences and Materials Systems Laboratory, General Motors, Warren, Michigan 489 University of Michigan Current address: Department of Chemistry and Chemical Engineering, Royal Military College of Canada, Kingston, Ontario, Canada K7K 7B4. General Motors Contents I II. III. IV Linker synthetic scheme TGA data Powder XRD patterns BET and Langmuir surface areas for UMCM-152 and UMCM-153 V. Ar isotherms and pore size distributions of UMCM-152 and UMCM-153 VI. Crystallographic tables 1
2 I. Linker synthetic scheme Synthesis of H 3-2 Synthesis of H 4-3 and H 5-4 2
3 weight (%) weight (%) weight (%) weight (%) II. TGA data Measurements were performed on a TA Q5 TGA apparatus. Approximately 1 mg of acetone or CH 2 Cl 2 exchanged material was loaded onto a platinum pan and excess solvent was allowed to evaporate to yield a free flowing powder before starting a temperature programmed ramp. Conditions: temperature ramp from 3 5 C at 5 C/min under a flow of N 2 gas. 1 a 1 b Temperature ( C) Temperature ( C) 1 c 1 d Temperature ( C) Temperature ( C) Figure S1: TGA traces of (a) UMCM-151, (b) UMCM-152, (c) UMCM-153, and (d) UMCM
4 Intensity (a.u.) III. Powder XRD patterns Powder X-ray diffraction was performed on a Rigaku R-Axis Spider diffractometer with an image plate detector and Cu Kα radiation operating in transmission mode. The sample was rotated in φ and oscillated in ω to minimize preferred orientation. a b c d Figure S2: As-synthesized and simulated PXRD patterns for (a) UMCM-151, (b) UMCM-152, (c) UMCM-153, and (d) UMCM
5 (P/Po)/W (g/g) 1/(W((Po/P)-1)) IV. BET and Langmuir surface areas for UMCM-152 and UMCM y = ax + b a =.9999 b =.5 R 2 = P/P o Figure S3: BET plot of the N 2 isotherm for UMCM-152 collected at 77 K y = ax + b a =.947 b =.16 R 2 = P/Po Figure S4: Langmuir plot of the N 2 isotherm for UMCM-152 collected at 77 K. 5
6 (P/Po)W (g/g) 1/(W((Po/P)-1)) y = ax + b a = b =.3 R 2 = P/Po Figure S5: BET plot of the N 2 isotherm for UMCM-153 collected at 77 K P/Po y = ax + b a =.932 b =.14 R 2 =.9999 Figure S6: Langmuir plot of the N 2 isotherm for UMCM-153 collected at 77 K. 6
7 Surface Area (m 2 /g) Ar Uptake (cc/g) V. Ar isotherms and pore size distributions of UMCM-152 and UMCM ads des fit P/Po Figure S7: Ar sorption isotherm at 87 K for UMCM-152 and the corresponding NLDFT fit based on a cylindrical pore model Pore Size (Å) Figure S8: Pore size distribution of UMCM
8 Surface Area (m 2 /g) Ar Uptake (cc/g) ads des fit P/Po Figure S9: Ar sorption isotherm at 87 K for UMCM-153 and the corresponding NLDFT fit based on a cylindrical pore model Pore Size (Å) Figure S1. Pore size distribution of UMCM
9 VI. Crystallographic Tables UMCM-151 Empirical formula C 42 H 22 O 15 Cu 3 Formula weight Temperature 253 K Wavelength Crystal System orthorhombic Space Group Immm (#71) Unit Cell Dimensions a = (17) Å α = 9º b = (2) Å β = 9º c = (2) Å γ = 9º Volume 27237(2) Å 3 Z 8 Density (calculated).467 g/cm 3 Absorption coefficient.727 mm -1 F() 3848 Crystal Size mm 3 Theta range for data collection 8.72 to 7.17 Index ranges h 28, k 37, l 38 Reflections collected Independent reflections 5264 [R(int) =.235]] Completeness to theta = % Absorption correction Empirical from equivalents Max. and min. transmission.8987 and.8114 Refinement method Full-matrix least-squares on F 2 Data / restraints / parameters 5264 / / 288 GOF on F Final R indices [I>2sigma(I)] R1 =.1327 wr2 =.3493 R indices (all data) R1 =.1744 wr2 =.3785 Largest diff. peak and hole and e - /Å 3 9
10 UMCM-152 Empirical formula C 14 H 7 O 5 Cu 5 Formula weight Temperature 293 (2) K Wavelength Crystal System Trigonal Space Group R3m (#16) Unit Cell Dimensions a = (11) Å α = 9º b = (11) Å β = 9º c = (19) Å γ = 12º Volume (15) Å 3 Z 18 Density (calculated).598 g/cm 3 Absorption coefficient.932 mm -1 F() 288 Crystal Size mm 3 Theta range for data collection 6.73 to 5.31 Index ranges -25 h 19, -2 k 26, -26 l 21 Reflections collected 1156 Independent reflections 3479 [R(int) =.759]] Completeness to theta = % Absorption correction Empirical from equivalents Max. and min. transmission.9376 and.8963 Refinement method Full-matrix least-squares on F 2 Data / restraints / parameters 3479 / 1 / 193 GOF on F Final R indices [I>2sigma(I)] R1 =.555 wr2 =.144 R indices (all data) R1 =.681 wr2 =.1555 Largest diff. peak and hole.383 and -.53 e - /Å 3 1
11 UMCM-153 Empirical formula C 14 H 7 O 5 Cu Formula weight Temperature 15 (2) K Wavelength Crystal System orthorhombic Space Group Fddd (#7) Unit Cell Dimensions a = (7) Å α = 9º b = 29.72(11) Å β = 9º c = 43.7(3) Å γ = 9º Volume 27515(2) Å 3 Z 32 Density (calculated).616 g/cm 3 Absorption coefficient.96 mm -1 F() 512 Crystal Size mm 3 Theta range for data collection 6.51 to 5.42 Index ranges -17 h 21, -17 k 28, -43 l 28 Reflections collected 1577 Independent reflections 3591 [R(int) =.1197] Completeness to theta = % Absorption correction Empirical from equivalents Max. and min. transmission.9626 and.8166 Refinement method Full-matrix least-squares on F 2 Data / restraints / parameters 3591 / / 183 GOF on F Final R indices [I>2sigma(I)] R1 =.768 wr2 =.1949 R indices (all data) R1 =.164 wr2 =.288 Largest diff. peak and hole.811 and e - /Å 3 11
12 UMCM-154 Empirical formula C 29 H 13 O 1 Zn 2 Formula weight Temperature 95 (2) K Wavelength Crystal System Monoclinic Space Group C2/c (#15) Unit Cell Dimensions a = (2) Å α = 9.º b = 3.771(6) Å β = 9.983(6)º c = (12) Å γ = 9.º Volume (5) Å 3 Z 4 Density (calculated).68 g/cm 3 Absorption coefficient mm -1 F() 138 Crystal Size mm 3 Theta range for data collection 6.51 to Index ranges -12 h 14, -36 k 35, -17 l 2119 Reflections collected Independent reflections 5485 [R(int) =.426]] Completeness to theta = % Absorption correction Empirical from equivalents Max. and min. transmission.8654 and.5663 Refinement method Full-matrix least-squares on F 2 Data / restraints / parameters 5485 / / 188 GOF on F Final R indices [I>2sigma(I)] R1 =.724 wr2 =.258 R indices (all data) R1 =.85 wr2 =.282 Largest diff. peak and hole.69 and e - /Å 3 12
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