Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401935X/hb6059sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680401935X/hb6059Isup2.hkl |
CCDC reference: 251610
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.024
- wR factor = 0.087
- Data-to-parameter ratio = 17.8
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.94
Author Response: Due to the measurement of low intensity reflections some strong reflections are excluded by the dataprocessing package |
Alert level B PLAT415_ALERT_2_B Short Inter D-H..H-X HC2 .. H2 .. 2.09 Ang. PLAT733_ALERT_1_B Torsion Calc -54.64(8), Rep -54.64(2) ...... 4.44 su-Rat MO3 -MO2 -MO3 -MO1 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_B Torsion Calc 54.64(8), Rep 54.64(2) ...... 4.44 su-Rat MO1 -MO2 -MO3 -MO2 3.556 1.555 1.555 3.556
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 26.02 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 2926 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 3117 Completeness (_total/calc) 93.87% PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.94 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - Cl3 .. 5.25 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - Cl7 .. 8.86 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - Cl4 .. 5.27 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo3 - Cl2 .. 5.34 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo3 - Cl1_a .. 5.97 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo3 - Cl3_a .. 5.01 su PLAT431_ALERT_2_C Short Inter HL..A Contact Cl6 .. N2 .. 3.19 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl6 .. N2 .. 3.29 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl7 .. Cl8 .. 3.37 Ang. PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 183 CL3 -MO2 -CL1 -MO3 29.30 0.60 3.556 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 190 CL3 -MO2 -CL1 -MO1 -42.40 0.60 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 198 CL2 -MO1 -CL1 -MO2 39.50 0.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 205 CL2 -MO1 -CL1 -MO3 -32.90 0.50 1.555 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 212 CL3 -MO3 -CL2 -MO2 -35.20 0.50 3.556 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 219 CL3 -MO3 -CL2 -MO1 37.20 0.50 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 226 CL1 -MO1 -CL2 -MO2 32.80 0.50 1.555 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 233 CL1 -MO1 -CL2 -MO3 -39.50 0.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 238 CL4 -MO1 -CL3 -MO2 -29.80 0.60 1.555 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 245 CL4 -MO1 -CL3 -MO3 42.60 0.60 1.555 1.555 1.555 3.556 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 253 CL1 -MO3 -CL4 -MO2 39.50 0.60 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 260 CL1 -MO3 -CL4 -MO1 -32.60 0.60 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 266 CL2 -MO2 -CL4 -MO3 -32.40 0.50 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 273 CL2 -MO2 -CL4 -MO1 39.40 0.50 3.556 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 280 CL3 -MO1 -CL4 -MO3 29.90 0.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 287 CL3 -MO1 -CL4 -MO2 -42.70 0.60 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 PLAT732_ALERT_1_C Angle Calc 175.52(9), Rep 175.52(4) ...... 2.25 su-Rat CL4 -MO1 -CL3 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 175.21(9), Rep 175.21(4) ...... 2.25 su-Rat CL2 -MO1 -CL1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 133.72(9), Rep 133.72(4) ...... 2.25 su-Rat CL7 -MO1 -MO2 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 134.29(9), Rep 134.29(4) ...... 2.25 su-Rat CL5 -MO2 -MO1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 58.03(9), Rep 58.03(4) ...... 2.25 su-Rat CL4 -MO3 -MO2 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.51(9), Rep 1.51(3) ...... 3.00 su-Rat MO3 -MO1 -MO2 -CL2 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 176.75(9), Rep 176.75(4) ...... 2.25 su-Rat CL1 -MO1 -MO2 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.52(9), Rep -1.52(3) ...... 3.00 su-Rat MO3 -MO1 -MO2 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 53.02(9), Rep 53.01(4) ...... 2.25 su-Rat MO2 -MO1 -MO2 -CL3 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -176.53(9), Rep -176.54(4) ...... 2.25 su-Rat CL2 -MO1 -MO2 -CL1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -178.27(9), Rep -178.27(3) ...... 3.00 su-Rat MO3 -MO1 -MO2 -CL1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -123.73(9), Rep -123.73(4) ...... 2.25 su-Rat MO2 -MO1 -MO2 -CL1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 178.16(9), Rep 178.15(4) ...... 2.25 su-Rat MO3 -MO1 -MO2 -CL4 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -178.16(9), Rep -178.15(4) ...... 2.25 su-Rat CL4 -MO1 -MO2 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.61(9), Rep -1.61(3) ...... 3.00 su-Rat CL3 -MO1 -MO2 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -52.80(9), Rep -52.80(4) ...... 2.25 su-Rat CL2 -MO1 -MO2 -MO1 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 123.73(9), Rep 123.73(4) ...... 2.25 su-Rat CL1 -MO1 -MO2 -MO1 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -54.54(8), Rep -54.54(3) ...... 2.67 su-Rat MO3 -MO1 -MO2 -MO1 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.74(9), Rep 1.74(3) ...... 3.00 su-Rat CL2 -MO1 -MO2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 178.27(9), Rep 178.27(3) ...... 3.00 su-Rat CL1 -MO1 -MO2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 54.54(8), Rep 54.54(3) ...... 2.67 su-Rat MO2 -MO1 -MO2 -MO3 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -178.65(9), Rep -178.65(4) ...... 2.25 su-Rat MO2 -MO1 -MO3 -CL4 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 176.54(9), Rep 176.54(4) ...... 2.25 su-Rat CL1 -MO1 -MO3 -CL2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 178.20(9), Rep 178.20(3) ...... 3.00 su-Rat MO2 -MO1 -MO3 -CL2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.14(9), Rep -1.14(3) ...... 3.00 su-Rat MO2 -MO1 -MO3 -CL1 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -176.70(9), Rep -176.69(4) ...... 2.25 su-Rat CL2 -MO1 -MO3 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -0.16(9), Rep -0.15(4) ...... 2.25 su-Rat CL1 -MO1 -MO3 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.51(9), Rep 1.51(3) ...... 3.00 su-Rat MO2 -MO1 -MO3 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 178.65(9), Rep 178.65(4) ...... 2.25 su-Rat CL4 -MO1 -MO3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.17(9), Rep 1.17(4) ...... 2.25 su-Rat CL3 -MO1 -MO3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -178.20(9), Rep -178.20(3) ...... 3.00 su-Rat CL2 -MO1 -MO3 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.66(9), Rep -1.66(3) ...... 3.00 su-Rat CL1 -MO1 -MO3 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 123.93(9), Rep 123.93(4) ...... 2.25 su-Rat MO3 -MO2 -MO3 -CL4 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 178.56(9), Rep 178.56(3) ...... 3.00 su-Rat MO1 -MO2 -MO3 -CL4 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 176.69(9), Rep 176.68(4) ...... 2.25 su-Rat CL3 -MO2 -MO3 -CL2 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 52.97(9), Rep 52.97(4) ...... 2.25 su-Rat MO3 -MO2 -MO3 -CL2 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.74(9), Rep -1.74(3) ...... 3.00 su-Rat MO1 -MO2 -MO3 -CL2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -53.11(9), Rep -53.11(3) ...... 3.00 su-Rat MO3 -MO2 -MO3 -CL1 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.53(9), Rep 1.52(3) ...... 3.00 su-Rat MO1 -MO2 -MO3 -CL1 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -123.72(9), Rep -123.72(4) ...... 2.25 su-Rat MO3 -MO2 -MO3 -CL3 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -178.43(9), Rep -178.42(3) ...... 3.00 su-Rat MO1 -MO2 -MO3 -CL3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.39(9), Rep -1.39(3) ...... 3.00 su-Rat CL2 -MO2 -MO3 -MO1 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -178.56(9), Rep -178.56(3) ...... 3.00 su-Rat CL4 -MO2 -MO3 -MO1 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 178.42(9), Rep 178.42(3) ...... 3.00 su-Rat CL3 -MO2 -MO3 -MO1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.68(9), Rep 1.68(3) ...... 3.00 su-Rat CL1 -MO2 -MO3 -MO1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 54.71(8), Rep 54.71(3) ...... 2.67 su-Rat MO3 -MO2 -MO3 -MO1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 53.25(9), Rep 53.25(3) ...... 3.00 su-Rat CL2 -MO2 -MO3 -MO2 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 123.72(9), Rep 123.72(4) ...... 2.25 su-Rat CL3 -MO2 -MO3 -MO2 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -53.02(9), Rep -53.02(4) ...... 2.25 su-Rat CL1 -MO2 -MO3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -123.93(9), Rep -123.93(4) ...... 2.25 su-Rat CL4 -MO2 -MO3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -54.71(8), Rep -54.71(3) ...... 2.67 su-Rat MO1 -MO2 -MO3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.16(9), Rep 1.16(3) ...... 3.00 su-Rat MO1 -MO2 -CL1 -MO3 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.70(9), Rep -1.70(3) ...... 3.00 su-Rat MO3 -MO2 -CL1 -MO1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -143.11(9), Rep -143.11(4) ...... 2.25 su-Rat CL7 -MO1 -CL1 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -51.47(9), Rep -51.47(4) ...... 2.25 su-Rat CL4 -MO1 -CL1 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 124.06(9), Rep 124.06(4) ...... 2.25 su-Rat CL3 -MO1 -CL1 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.71(9), Rep 1.70(3) ...... 3.00 su-Rat MO3 -MO1 -CL1 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -123.83(9), Rep -123.83(4) ...... 2.25 su-Rat CL4 -MO1 -CL1 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 51.70(9), Rep 51.70(3) ...... 3.00 su-Rat CL3 -MO1 -CL1 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.54(9), Rep -1.54(3) ...... 3.00 su-Rat MO2 -MO1 -CL1 -MO3 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.54(9), Rep -1.53(3) ...... 3.00 su-Rat MO1 -MO3 -CL2 -MO2 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -51.55(9), Rep -51.55(4) ...... 2.25 su-Rat CL4 -MO3 -CL2 -MO1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 124.39(9), Rep 124.39(4) ...... 2.25 su-Rat CL1 -MO3 -CL2 -MO1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.77(9), Rep 1.77(3) ...... 3.00 su-Rat MO2 -MO3 -CL2 -MO1 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 123.77(9), Rep 123.77(4) ...... 2.25 su-Rat CL4 -MO1 -CL2 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -51.80(9), Rep -51.80(3) ...... 3.00 su-Rat CL3 -MO1 -CL2 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.41(9), Rep 1.42(3) ...... 3.00 su-Rat MO3 -MO1 -CL2 -MO2 3.556 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 143.09(9), Rep 143.09(4) ...... 2.25 su-Rat CL7 -MO1 -CL2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 51.43(9), Rep 51.43(4) ...... 2.25 su-Rat CL4 -MO1 -CL2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -124.13(9), Rep -124.14(4) ...... 2.25 su-Rat CL3 -MO1 -CL2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.78(9), Rep -1.78(3) ...... 3.00 su-Rat MO2 -MO1 -CL2 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 51.53(9), Rep 51.53(4) ...... 2.25 su-Rat CL2 -MO1 -CL3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -123.70(9), Rep -123.70(4) ...... 2.25 su-Rat CL1 -MO1 -CL3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -1.20(9), Rep -1.20(4) ...... 2.25 su-Rat MO3 -MO1 -CL3 -MO2 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 123.91(9), Rep 123.90(4) ...... 2.25 su-Rat CL2 -MO1 -CL3 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc -51.32(9), Rep -51.33(4) ...... 2.25 su-Rat CL1 -MO1 -CL3 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.64(9), Rep 1.64(3) ...... 3.00 su-Rat MO2 -MO1 -CL3 -MO3 1.555 1.555 1.555 3.556 PLAT733_ALERT_1_C Torsion Calc 1.41(9), Rep 1.41(3) ...... 3.00 su-Rat MO1 -MO3 -CL4 -MO2 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.34(9), Rep -1.34(4) ...... 2.25 su-Rat MO2 -MO3 -CL4 -MO1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.40(9), Rep -1.40(3) ...... 3.00 su-Rat MO1 -MO2 -CL4 -MO3 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.81(9), Rep 1.81(3) ...... 3.00 su-Rat MO3 -MO2 -CL4 -MO1 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -51.43(9), Rep -51.43(4) ...... 2.25 su-Rat CL2 -MO1 -CL4 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 123.78(9), Rep 123.78(4) ...... 2.25 su-Rat CL1 -MO1 -CL4 -MO3 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 1.33(9), Rep 1.33(3) ...... 3.00 su-Rat MO2 -MO1 -CL4 -MO3 3.556 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -123.97(9), Rep -123.97(4) ...... 2.25 su-Rat CL2 -MO1 -CL4 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc 51.24(9), Rep 51.24(4) ...... 2.25 su-Rat CL1 -MO1 -CL4 -MO2 1.555 1.555 1.555 1.555 PLAT733_ALERT_1_C Torsion Calc -1.81(9), Rep -1.81(3) ...... 3.00 su-Rat MO3 -MO1 -CL4 -MO2 3.556 1.555 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.24 Ratio
1 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 117 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 90 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 18 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS (Stoe & Cie, 1997); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) and JANA2000 (Petříček & Dušek, 2000); program(s) used to refine structure: SHELXL97 and JANA2000; software used to prepare material for publication: SHELXL97 and JANA2000.
(C5H6ClN2)2[Mo6Cl14] | F(000) = 1248 |
Mr = 1331.08 | Dx = 2.794 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5000 reflections |
a = 9.186 (6) Å | θ = 4.3–52.0° |
b = 18.238 (8) Å | µ = 3.67 mm−1 |
c = 9.614 (6) Å | T = 293 K |
β = 100.81 (8)° | Block, yellow |
V = 1582.0 (16) Å3 | 0.18 × 0.18 × 0.10 mm |
Z = 2 |
Stoe IPDS CCD area-detector diffractometer | 2926 independent reflections |
Radiation source: fine-focus sealed tube | 2486 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
φ scans | θmax = 26.0°, θmin = 2.2° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996) | h = −10→10 |
Tmin = 0.486, Tmax = 0.652 | k = −22→22 |
12075 measured reflections | l = −11→11 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F > 3σ(F)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F) = 0.087 | H-atom parameters constrained |
S = 1.18 | w = 1/[σ2(Fo2) + (0.052P)2] where P = (Fo2 + 2Fc2)/3 |
2926 reflections | (Δ/σ)max = 0.001 |
164 parameters | Δρmax = 1.04 e Å−3 |
68 restraints | Δρmin = −1.64 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | −0.00010 (4) | 0.100068 (18) | 0.47496 (4) | 0.01963 (12) | |
Mo2 | −0.15957 (4) | 0.008489 (19) | 0.59196 (4) | 0.01913 (12) | |
Mo3 | 0.12952 (4) | 0.010232 (19) | 0.67028 (4) | 0.01948 (13) | |
Cl1 | −0.27502 (13) | 0.09267 (6) | 0.40153 (12) | 0.0265 (3) | |
Cl2 | 0.27330 (13) | 0.09608 (6) | 0.54957 (12) | 0.0264 (2) | |
Cl3 | 0.02950 (14) | 0.07736 (6) | 0.22789 (11) | 0.0275 (3) | |
Cl4 | −0.02736 (14) | 0.11232 (6) | 0.72522 (11) | 0.0268 (3) | |
Cl5 | −0.36865 (15) | 0.02181 (7) | 0.71410 (13) | 0.0336 (3) | |
Cl6 | 0.29550 (15) | 0.02352 (7) | 0.89955 (12) | 0.0341 (3) | |
Cl7 | −0.00424 (16) | 0.23201 (6) | 0.44373 (16) | 0.0412 (3) | |
C1 | 0.6433 (6) | 0.1754 (3) | 0.0559 (5) | 0.0312 (11) | |
N1 | 0.7421 (6) | 0.1478 (2) | −0.0160 (5) | 0.0438 (12) | |
H1 | 0.8149 | 0.1800 | −0.0159 | 0.066* | |
H2 | 0.6978 | 0.1387 | −0.1049 | 0.066* | |
H3 | 0.7794 | 0.1064 | 0.0248 | 0.066* | |
C2 | 0.5487 (7) | 0.2714 (3) | 0.1831 (6) | 0.0401 (13) | |
HC2 | 0.5543 | 0.3190 | 0.2186 | 0.060* | |
C3 | 0.4310 (6) | 0.2253 (3) | 0.2031 (5) | 0.0348 (12) | |
C4 | 0.6533 (7) | 0.2467 (3) | 0.1127 (6) | 0.0380 (13) | |
HC4 | 0.7320 | 0.2769 | 0.1018 | 0.057* | |
C5 | 0.4224 (7) | 0.1583 (3) | 0.1480 (6) | 0.0397 (13) | |
HC5 | 0.3444 | 0.1276 | 0.1586 | 0.060* | |
N2 | 0.5279 (5) | 0.1345 (2) | 0.0760 (5) | 0.0374 (11) | |
Cl8 | 0.2997 (2) | 0.25423 (9) | 0.29898 (18) | 0.0551 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0220 (3) | 0.01440 (19) | 0.0218 (2) | 0.00112 (13) | 0.00252 (15) | 0.00001 (13) |
Mo2 | 0.0202 (3) | 0.0170 (2) | 0.0199 (2) | 0.00098 (13) | 0.00308 (15) | −0.00076 (13) |
Mo3 | 0.0208 (3) | 0.0178 (2) | 0.0184 (2) | 0.00063 (13) | −0.00003 (15) | −0.00126 (13) |
Cl1 | 0.0244 (7) | 0.0250 (5) | 0.0284 (6) | 0.0060 (4) | 0.0005 (4) | 0.0018 (4) |
Cl2 | 0.0242 (7) | 0.0230 (5) | 0.0311 (6) | −0.0040 (4) | 0.0024 (4) | −0.0026 (4) |
Cl3 | 0.0317 (7) | 0.0276 (5) | 0.0229 (5) | 0.0008 (4) | 0.0042 (4) | 0.0054 (4) |
Cl4 | 0.0317 (7) | 0.0222 (5) | 0.0262 (5) | 0.0014 (4) | 0.0049 (4) | −0.0065 (4) |
Cl5 | 0.0304 (8) | 0.0370 (6) | 0.0363 (6) | 0.0026 (5) | 0.0140 (5) | −0.0007 (5) |
Cl6 | 0.0375 (8) | 0.0327 (6) | 0.0266 (6) | −0.0031 (5) | −0.0079 (5) | −0.0043 (5) |
Cl7 | 0.0469 (9) | 0.0191 (5) | 0.0618 (9) | −0.0053 (5) | 0.0212 (6) | −0.0081 (5) |
C1 | 0.032 (3) | 0.027 (2) | 0.033 (3) | −0.0044 (19) | −0.001 (2) | 0.0031 (19) |
N1 | 0.048 (3) | 0.033 (2) | 0.050 (3) | −0.002 (2) | 0.011 (2) | 0.000 (2) |
C2 | 0.050 (4) | 0.028 (3) | 0.040 (3) | −0.009 (2) | 0.003 (3) | −0.002 (2) |
C3 | 0.039 (3) | 0.031 (3) | 0.033 (3) | 0.002 (2) | 0.002 (2) | 0.005 (2) |
C4 | 0.044 (4) | 0.029 (3) | 0.040 (3) | −0.015 (2) | 0.006 (2) | 0.000 (2) |
C5 | 0.038 (4) | 0.029 (3) | 0.052 (3) | −0.009 (2) | 0.006 (3) | 0.004 (2) |
N2 | 0.038 (3) | 0.023 (2) | 0.052 (3) | −0.0099 (17) | 0.008 (2) | −0.0039 (18) |
Cl8 | 0.0598 (12) | 0.0575 (9) | 0.0526 (9) | −0.0097 (7) | 0.0220 (7) | −0.0053 (7) |
Mo1—Mo3i | 2.6052 (13) | Mo3—Cl2 | 2.4732 (16) |
Mo1—Mo3 | 2.6057 (15) | Mo3—Cl1i | 2.4761 (15) |
Mo1—Mo2 | 2.6112 (13) | Mo3—Cl3i | 2.4860 (16) |
Mo1—Mo2i | 2.6151 (11) | Cl1—Mo3i | 2.4761 (15) |
Mo2—Mo3 | 2.621 (2) | Cl2—Mo2i | 2.4590 (16) |
Mo2—Mo3i | 2.6096 (17) | Cl3—Mo2i | 2.4703 (18) |
Mo2—Mo1i | 2.6151 (11) | Cl3—Mo3i | 2.4860 (16) |
Mo3—Mo1i | 2.6052 (13) | C1—N1 | 1.338 (7) |
Mo3—Mo2i | 2.6096 (17) | C1—N2 | 1.339 (7) |
Mo1—Cl7 | 2.4243 (16) | C1—C4 | 1.407 (7) |
Mo1—Cl4 | 2.4754 (19) | N1—H1 | 0.8900 |
Mo1—Cl3 | 2.4757 (19) | N1—H2 | 0.8900 |
Mo1—Cl2 | 2.480 (2) | N1—H3 | 0.8900 |
Mo1—Cl1 | 2.495 (2) | C2—C4 | 1.353 (8) |
Mo2—Cl5 | 2.444 (2) | C2—C3 | 1.411 (8) |
Mo2—Cl2i | 2.4590 (16) | C2—HC2 | 0.9300 |
Mo2—Cl3i | 2.4703 (18) | C3—C5 | 1.327 (7) |
Mo2—Cl1 | 2.4709 (17) | C3—Cl8 | 1.732 (6) |
Mo2—Cl4 | 2.4735 (16) | C4—HC4 | 0.9300 |
Mo3—Cl6 | 2.446 (2) | C5—N2 | 1.364 (8) |
Mo3—Cl4 | 2.4713 (15) | C5—HC5 | 0.9300 |
Cl7—Mo1—Cl4 | 91.64 (5) | Mo1i—Mo2—Mo3 | 59.68 (3) |
Cl7—Mo1—Cl3 | 92.82 (5) | Cl6—Mo3—Cl4 | 91.30 (6) |
Cl4—Mo1—Cl3 | 175.52 (4) | Cl6—Mo3—Cl2 | 93.59 (6) |
Cl7—Mo1—Cl2 | 93.24 (5) | Cl4—Mo3—Cl2 | 90.43 (6) |
Cl4—Mo1—Cl2 | 90.17 (9) | Cl6—Mo3—Cl1i | 92.78 (6) |
Cl3—Mo1—Cl2 | 89.15 (8) | Cl4—Mo3—Cl1i | 175.92 (4) |
Cl7—Mo1—Cl1 | 91.55 (5) | Cl2—Mo3—Cl1i | 89.16 (6) |
Cl4—Mo1—Cl1 | 89.91 (9) | Cl6—Mo3—Cl3i | 91.25 (6) |
Cl3—Mo1—Cl1 | 90.40 (8) | Cl4—Mo3—Cl3i | 89.47 (6) |
Cl2—Mo1—Cl1 | 175.21 (4) | Cl2—Mo3—Cl3i | 175.16 (4) |
Cl7—Mo1—Mo3i | 134.83 (5) | Cl1i—Mo3—Cl3i | 90.60 (6) |
Cl4—Mo1—Mo3i | 118.13 (5) | Cl6—Mo3—Mo1i | 134.77 (4) |
Cl3—Mo1—Mo3i | 58.52 (4) | Cl4—Mo3—Mo1i | 118.07 (5) |
Cl2—Mo1—Mo3i | 117.90 (5) | Cl2—Mo3—Mo1i | 117.87 (5) |
Cl1—Mo1—Mo3i | 58.04 (5) | Cl1i—Mo3—Mo1i | 58.75 (5) |
Cl7—Mo1—Mo3 | 135.05 (5) | Cl3i—Mo3—Mo1i | 58.14 (5) |
Cl4—Mo1—Mo3 | 58.14 (5) | Cl6—Mo3—Mo1 | 135.28 (5) |
Cl3—Mo1—Mo3 | 117.95 (5) | Cl4—Mo3—Mo1 | 58.29 (5) |
Cl2—Mo1—Mo3 | 58.13 (6) | Cl2—Mo3—Mo1 | 58.39 (5) |
Cl1—Mo1—Mo3 | 118.12 (6) | Cl1i—Mo3—Mo1 | 118.25 (5) |
Mo3i—Mo1—Mo3 | 90.09 (6) | Cl3i—Mo3—Mo1 | 117.71 (5) |
Cl7—Mo1—Mo2 | 133.72 (4) | Mo1i—Mo3—Mo1 | 89.91 (6) |
Cl4—Mo1—Mo2 | 58.12 (5) | Cl6—Mo3—Mo2i | 136.28 (6) |
Cl3—Mo1—Mo2 | 118.54 (5) | Cl4—Mo3—Mo2i | 118.46 (5) |
Cl2—Mo1—Mo2 | 118.43 (5) | Cl2—Mo3—Mo2i | 57.79 (5) |
Cl1—Mo1—Mo2 | 57.83 (5) | Cl1i—Mo3—Mo2i | 58.07 (5) |
Mo3i—Mo1—Mo2 | 60.03 (4) | Cl3i—Mo3—Mo2i | 118.21 (5) |
Mo3—Mo1—Mo2 | 60.32 (4) | Mo1i—Mo3—Mo2i | 60.10 (4) |
Cl7—Mo1—Mo2i | 135.85 (5) | Mo1—Mo3—Mo2i | 60.19 (4) |
Cl4—Mo1—Mo2i | 118.10 (5) | Cl6—Mo3—Mo2 | 133.39 (7) |
Cl3—Mo1—Mo2i | 57.98 (5) | Cl4—Mo3—Mo2 | 58.03 (4) |
Cl2—Mo1—Mo2i | 57.64 (4) | Cl2—Mo3—Mo2 | 118.31 (5) |
Cl1—Mo1—Mo2i | 118.30 (4) | Cl1i—Mo3—Mo2 | 118.78 (4) |
Mo3i—Mo1—Mo2i | 60.27 (4) | Cl3i—Mo3—Mo2 | 57.78 (5) |
Mo3—Mo1—Mo2i | 59.98 (4) | Mo1i—Mo3—Mo2 | 60.05 (4) |
Mo2—Mo1—Mo2i | 90.43 (5) | Mo1—Mo3—Mo2 | 59.95 (5) |
Cl5—Mo2—Cl2i | 93.00 (6) | Mo2i—Mo3—Mo2 | 90.34 (8) |
Cl5—Mo2—Cl3i | 92.66 (6) | Mo2—Cl1—Mo3i | 63.67 (5) |
Cl2i—Mo2—Cl3i | 89.76 (7) | Mo2—Cl1—Mo1 | 63.45 (6) |
Cl5—Mo2—Cl1 | 91.58 (6) | Mo3i—Cl1—Mo1 | 63.21 (4) |
Cl2i—Mo2—Cl1 | 89.61 (7) | Mo2i—Cl2—Mo3 | 63.89 (5) |
Cl3i—Mo2—Cl1 | 175.74 (4) | Mo2i—Cl2—Mo1 | 63.94 (5) |
Cl5—Mo2—Cl4 | 91.65 (6) | Mo3—Cl2—Mo1 | 63.48 (5) |
Cl2i—Mo2—Cl4 | 175.34 (4) | Mo2i—Cl3—Mo1 | 63.84 (5) |
Cl3i—Mo2—Cl4 | 89.78 (7) | Mo2i—Cl3—Mo3i | 63.85 (5) |
Cl1—Mo2—Cl4 | 90.51 (7) | Mo1—Cl3—Mo3i | 63.34 (5) |
Cl5—Mo2—Mo3i | 135.42 (6) | Mo3—Cl4—Mo2 | 64.02 (5) |
Cl2i—Mo2—Mo3i | 58.32 (4) | Mo3—Cl4—Mo1 | 63.57 (5) |
Cl3i—Mo2—Mo3i | 118.00 (5) | Mo2—Cl4—Mo1 | 63.69 (5) |
Cl1—Mo2—Mo3i | 58.26 (5) | N1—C1—N2 | 119.9 (5) |
Cl4—Mo2—Mo3i | 118.03 (5) | N1—C1—C4 | 123.1 (5) |
Cl5—Mo2—Mo1 | 134.29 (4) | N2—C1—C4 | 117.0 (5) |
Cl2i—Mo2—Mo1 | 118.17 (5) | C1—N1—H1 | 109.5 |
Cl3i—Mo2—Mo1 | 118.09 (5) | C1—N1—H2 | 109.5 |
Cl1—Mo2—Mo1 | 58.73 (5) | H1—N1—H2 | 109.5 |
Cl4—Mo2—Mo1 | 58.19 (5) | C1—N1—H3 | 109.5 |
Mo3i—Mo2—Mo1 | 59.87 (4) | H1—N1—H3 | 109.5 |
Cl5—Mo2—Mo1i | 136.14 (4) | H2—N1—H3 | 109.5 |
Cl2i—Mo2—Mo1i | 58.43 (5) | C4—C2—C3 | 120.2 (5) |
Cl3i—Mo2—Mo1i | 58.18 (5) | C4—C2—HC2 | 119.9 |
Cl1—Mo2—Mo1i | 118.08 (5) | C3—C2—HC2 | 119.9 |
Cl4—Mo2—Mo1i | 117.61 (5) | C5—C3—C2 | 119.0 (5) |
Mo3i—Mo2—Mo1i | 59.83 (4) | C5—C3—Cl8 | 119.8 (5) |
Mo1—Mo2—Mo1i | 89.57 (5) | C2—C3—Cl8 | 121.2 (4) |
Cl5—Mo2—Mo3 | 134.91 (5) | C2—C4—C1 | 120.1 (5) |
Cl2i—Mo2—Mo3 | 118.09 (5) | C2—C4—HC4 | 119.9 |
Cl3i—Mo2—Mo3 | 58.37 (6) | C1—C4—HC4 | 119.9 |
Cl1—Mo2—Mo3 | 118.44 (6) | C3—C5—N2 | 120.1 (5) |
Cl4—Mo2—Mo3 | 57.95 (5) | C3—C5—HC5 | 120.0 |
Mo3i—Mo2—Mo3 | 89.66 (8) | N2—C5—HC5 | 120.0 |
Mo1—Mo2—Mo3 | 59.74 (4) | C1—N2—C5 | 123.6 (4) |
Cl7—Mo1—Mo2—Cl5 | −0.67 (8) | Cl5—Mo2—Mo3—Cl3i | 57.53 (6) |
Cl4—Mo1—Mo2—Cl5 | 56.09 (7) | Cl2i—Mo2—Mo3—Cl3i | −70.47 (6) |
Cl3—Mo1—Mo2—Cl5 | −127.36 (7) | Cl1—Mo2—Mo3—Cl3i | −176.74 (5) |
Cl2—Mo1—Mo2—Cl5 | 126.67 (6) | Cl4—Mo2—Mo3—Cl3i | 112.36 (6) |
Cl1—Mo1—Mo2—Cl5 | −56.80 (6) | Mo3i—Mo2—Mo3—Cl3i | −123.72 (4) |
Mo3i—Mo1—Mo2—Cl5 | −125.75 (7) | Mo1—Mo2—Mo3—Cl3i | −178.42 (3) |
Mo3—Mo1—Mo2—Cl5 | 124.93 (6) | Mo1i—Mo2—Mo3—Cl3i | −69.08 (5) |
Mo2i—Mo1—Mo2—Cl5 | 179.47 (5) | Cl5—Mo2—Mo3—Mo1i | 126.61 (5) |
Cl7—Mo1—Mo2—Cl2i | 126.59 (8) | Cl2i—Mo2—Mo3—Mo1i | −1.39 (3) |
Cl4—Mo1—Mo2—Cl2i | −176.65 (5) | Cl3i—Mo2—Mo3—Mo1i | 69.08 (5) |
Cl3—Mo1—Mo2—Cl2i | −0.10 (5) | Cl1—Mo2—Mo3—Mo1i | −107.66 (5) |
Cl2—Mo1—Mo2—Cl2i | −106.07 (7) | Cl4—Mo2—Mo3—Mo1i | −178.56 (3) |
Cl1—Mo1—Mo2—Cl2i | 70.46 (7) | Mo3i—Mo2—Mo3—Mo1i | −54.637 (18) |
Mo3i—Mo1—Mo2—Cl2i | 1.51 (3) | Mo1—Mo2—Mo3—Mo1i | −109.34 (4) |
Mo3—Mo1—Mo2—Cl2i | −107.81 (7) | Cl5—Mo2—Mo3—Mo1 | −124.05 (6) |
Mo2i—Mo1—Mo2—Cl2i | −53.27 (6) | Cl2i—Mo2—Mo3—Mo1 | 107.95 (5) |
Cl7—Mo1—Mo2—Cl3i | −127.12 (7) | Cl3i—Mo2—Mo3—Mo1 | 178.42 (3) |
Cl4—Mo1—Mo2—Cl3i | −70.36 (7) | Cl1—Mo2—Mo3—Mo1 | 1.68 (3) |
Cl3—Mo1—Mo2—Cl3i | 106.18 (7) | Cl4—Mo2—Mo3—Mo1 | −69.22 (5) |
Cl2—Mo1—Mo2—Cl3i | 0.21 (5) | Mo3i—Mo2—Mo3—Mo1 | 54.71 (3) |
Cl1—Mo1—Mo2—Cl3i | 176.75 (4) | Mo1i—Mo2—Mo3—Mo1 | 109.34 (4) |
Mo3i—Mo1—Mo2—Cl3i | 107.79 (7) | Cl5—Mo2—Mo3—Mo2i | −178.76 (5) |
Mo3—Mo1—Mo2—Cl3i | −1.52 (3) | Cl2i—Mo2—Mo3—Mo2i | 53.25 (3) |
Mo2i—Mo1—Mo2—Cl3i | 53.01 (4) | Cl3i—Mo2—Mo3—Mo2i | 123.72 (4) |
Cl7—Mo1—Mo2—Cl1 | 56.13 (7) | Cl1—Mo2—Mo3—Mo2i | −53.02 (4) |
Cl4—Mo1—Mo2—Cl1 | 112.89 (7) | Cl4—Mo2—Mo3—Mo2i | −123.93 (4) |
Cl3—Mo1—Mo2—Cl1 | −70.57 (7) | Mo3i—Mo2—Mo3—Mo2i | 0.0 |
Cl2—Mo1—Mo2—Cl1 | −176.54 (4) | Mo1—Mo2—Mo3—Mo2i | −54.71 (3) |
Mo3i—Mo1—Mo2—Cl1 | −68.95 (6) | Mo1i—Mo2—Mo3—Mo2i | 54.637 (18) |
Mo3—Mo1—Mo2—Cl1 | −178.27 (3) | Cl5—Mo2—Cl1—Mo3i | −145.17 (5) |
Mo2i—Mo1—Mo2—Cl1 | −123.73 (4) | Cl2i—Mo2—Cl1—Mo3i | −52.18 (5) |
Cl7—Mo1—Mo2—Cl4 | −56.76 (8) | Cl3i—Mo2—Cl1—Mo3i | 29.3 (6) |
Cl3—Mo1—Mo2—Cl4 | 176.54 (5) | Cl4—Mo2—Cl1—Mo3i | 123.17 (5) |
Cl2—Mo1—Mo2—Cl4 | 70.57 (7) | Mo1—Mo2—Cl1—Mo3i | 71.64 (6) |
Cl1—Mo1—Mo2—Cl4 | −112.89 (7) | Mo1i—Mo2—Cl1—Mo3i | 1.16 (3) |
Mo3i—Mo1—Mo2—Cl4 | 178.15 (4) | Mo3—Mo2—Cl1—Mo3i | 69.95 (6) |
Mo3—Mo1—Mo2—Cl4 | 68.84 (7) | Cl5—Mo2—Cl1—Mo1 | 143.19 (5) |
Mo2i—Mo1—Mo2—Cl4 | 123.37 (6) | Cl2i—Mo2—Cl1—Mo1 | −123.82 (5) |
Cl7—Mo1—Mo2—Mo3i | 125.08 (7) | Cl3i—Mo2—Cl1—Mo1 | −42.4 (6) |
Cl4—Mo1—Mo2—Mo3i | −178.15 (4) | Cl4—Mo2—Cl1—Mo1 | 51.53 (5) |
Cl3—Mo1—Mo2—Mo3i | −1.61 (3) | Mo3i—Mo2—Cl1—Mo1 | −71.64 (6) |
Cl2—Mo1—Mo2—Mo3i | −107.58 (7) | Mo1i—Mo2—Cl1—Mo1 | −70.48 (6) |
Cl1—Mo1—Mo2—Mo3i | 68.95 (6) | Mo3—Mo2—Cl1—Mo1 | −1.70 (3) |
Mo3—Mo1—Mo2—Mo3i | −109.32 (6) | Cl7—Mo1—Cl1—Mo2 | −143.11 (4) |
Mo2i—Mo1—Mo2—Mo3i | −54.78 (5) | Cl4—Mo1—Cl1—Mo2 | −51.47 (4) |
Cl7—Mo1—Mo2—Mo1i | 179.86 (6) | Cl3—Mo1—Cl1—Mo2 | 124.06 (4) |
Cl4—Mo1—Mo2—Mo1i | −123.37 (6) | Cl2—Mo1—Cl1—Mo2 | 39.5 (5) |
Cl3—Mo1—Mo2—Mo1i | 53.17 (6) | Mo3i—Mo1—Cl1—Mo2 | 72.36 (5) |
Cl2—Mo1—Mo2—Mo1i | −52.80 (4) | Mo3—Mo1—Cl1—Mo2 | 1.70 (3) |
Cl1—Mo1—Mo2—Mo1i | 123.73 (4) | Mo2i—Mo1—Cl1—Mo2 | 70.82 (5) |
Mo3i—Mo1—Mo2—Mo1i | 54.78 (5) | Cl7—Mo1—Cl1—Mo3i | 144.53 (5) |
Mo3—Mo1—Mo2—Mo1i | −54.54 (3) | Cl4—Mo1—Cl1—Mo3i | −123.83 (4) |
Mo2i—Mo1—Mo2—Mo1i | 0.0 | Cl3—Mo1—Cl1—Mo3i | 51.70 (3) |
Cl7—Mo1—Mo2—Mo3 | −125.60 (6) | Cl2—Mo1—Cl1—Mo3i | −32.9 (5) |
Cl4—Mo1—Mo2—Mo3 | −68.84 (7) | Mo3—Mo1—Cl1—Mo3i | −70.66 (5) |
Cl3—Mo1—Mo2—Mo3 | 107.71 (7) | Mo2—Mo1—Cl1—Mo3i | −72.36 (5) |
Cl2—Mo1—Mo2—Mo3 | 1.74 (3) | Mo2i—Mo1—Cl1—Mo3i | −1.54 (3) |
Cl1—Mo1—Mo2—Mo3 | 178.27 (3) | Cl6—Mo3—Cl2—Mo2i | 144.71 (5) |
Mo3i—Mo1—Mo2—Mo3 | 109.32 (6) | Cl4—Mo3—Cl2—Mo2i | −123.96 (6) |
Mo2i—Mo1—Mo2—Mo3 | 54.54 (3) | Cl1i—Mo3—Cl2—Mo2i | 51.98 (6) |
Cl7—Mo1—Mo3—Cl6 | 0.79 (8) | Cl3i—Mo3—Cl2—Mo2i | −35.2 (5) |
Cl4—Mo1—Mo3—Cl6 | −54.12 (7) | Mo1i—Mo3—Cl2—Mo2i | −1.53 (3) |
Cl3—Mo1—Mo3—Cl6 | 128.41 (7) | Mo1—Mo3—Cl2—Mo2i | −72.41 (6) |
Cl2—Mo1—Mo3—Cl6 | 58.87 (7) | Mo2—Mo3—Cl2—Mo2i | −70.64 (6) |
Cl1—Mo1—Mo3—Cl6 | −124.59 (7) | Cl6—Mo3—Cl2—Mo1 | −142.88 (5) |
Mo3i—Mo1—Mo3—Cl6 | −177.77 (6) | Cl4—Mo3—Cl2—Mo1 | −51.55 (4) |
Mo2—Mo1—Mo3—Cl6 | −122.93 (7) | Cl1i—Mo3—Cl2—Mo1 | 124.39 (4) |
Mo2i—Mo1—Mo3—Cl6 | 127.23 (6) | Cl3i—Mo3—Cl2—Mo1 | 37.2 (5) |
Cl7—Mo1—Mo3—Cl4 | 54.91 (7) | Mo1i—Mo3—Cl2—Mo1 | 70.88 (6) |
Cl3—Mo1—Mo3—Cl4 | −177.47 (5) | Mo2i—Mo3—Cl2—Mo1 | 72.41 (6) |
Cl2—Mo1—Mo3—Cl4 | 112.99 (7) | Mo2—Mo3—Cl2—Mo1 | 1.77 (3) |
Cl1—Mo1—Mo3—Cl4 | −70.47 (7) | Cl7—Mo1—Cl2—Mo2i | −144.58 (5) |
Mo3i—Mo1—Mo3—Cl4 | −123.65 (5) | Cl4—Mo1—Cl2—Mo2i | 123.77 (4) |
Mo2—Mo1—Mo3—Cl4 | −68.81 (6) | Cl3—Mo1—Cl2—Mo2i | −51.80 (3) |
Mo2i—Mo1—Mo3—Cl4 | −178.65 (4) | Cl1—Mo1—Cl2—Mo2i | 32.8 (5) |
Cl7—Mo1—Mo3—Cl2 | −58.08 (7) | Mo3i—Mo1—Cl2—Mo2i | 1.42 (3) |
Cl4—Mo1—Mo3—Cl2 | −112.99 (7) | Mo3—Mo1—Cl2—Mo2i | 72.33 (5) |
Cl3—Mo1—Mo3—Cl2 | 69.54 (7) | Mo2—Mo1—Cl2—Mo2i | 70.56 (5) |
Cl1—Mo1—Mo3—Cl2 | 176.54 (4) | Cl7—Mo1—Cl2—Mo3 | 143.09 (4) |
Mo3i—Mo1—Mo3—Cl2 | 123.36 (5) | Cl4—Mo1—Cl2—Mo3 | 51.43 (4) |
Mo2—Mo1—Mo3—Cl2 | 178.20 (3) | Cl3—Mo1—Cl2—Mo3 | −124.14 (4) |
Mo2i—Mo1—Mo3—Cl2 | 68.36 (6) | Cl1—Mo1—Cl2—Mo3 | −39.5 (5) |
Cl7—Mo1—Mo3—Cl1i | −127.58 (7) | Mo3i—Mo1—Cl2—Mo3 | −70.92 (5) |
Cl4—Mo1—Mo3—Cl1i | 177.51 (5) | Mo2—Mo1—Cl2—Mo3 | −1.78 (3) |
Cl3—Mo1—Mo3—Cl1i | 0.03 (5) | Mo2i—Mo1—Cl2—Mo3 | −72.33 (5) |
Cl2—Mo1—Mo3—Cl1i | −69.50 (7) | Cl7—Mo1—Cl3—Mo2i | 144.73 (5) |
Cl1—Mo1—Mo3—Cl1i | 107.04 (7) | Cl4—Mo1—Cl3—Mo2i | −29.8 (6) |
Mo3i—Mo1—Mo3—Cl1i | 53.86 (5) | Cl2—Mo1—Cl3—Mo2i | 51.53 (4) |
Mo2—Mo1—Mo3—Cl1i | 108.70 (6) | Cl1—Mo1—Cl3—Mo2i | −123.70 (4) |
Mo2i—Mo1—Mo3—Cl1i | −1.14 (3) | Mo3i—Mo1—Cl3—Mo2i | −72.37 (5) |
Cl7—Mo1—Mo3—Cl3i | 125.22 (7) | Mo3—Mo1—Cl3—Mo2i | −1.20 (4) |
Cl4—Mo1—Mo3—Cl3i | 70.32 (7) | Mo2—Mo1—Cl3—Mo2i | −70.74 (6) |
Cl3—Mo1—Mo3—Cl3i | −107.16 (7) | Cl7—Mo1—Cl3—Mo3i | −142.90 (5) |
Cl2—Mo1—Mo3—Cl3i | −176.69 (4) | Cl4—Mo1—Cl3—Mo3i | 42.6 (6) |
Cl1—Mo1—Mo3—Cl3i | −0.15 (4) | Cl2—Mo1—Cl3—Mo3i | 123.90 (4) |
Mo3i—Mo1—Mo3—Cl3i | −53.33 (5) | Cl1—Mo1—Cl3—Mo3i | −51.33 (4) |
Mo2—Mo1—Mo3—Cl3i | 1.51 (3) | Mo3—Mo1—Cl3—Mo3i | 71.17 (6) |
Mo2i—Mo1—Mo3—Cl3i | −108.33 (6) | Mo2—Mo1—Cl3—Mo3i | 1.64 (3) |
Cl7—Mo1—Mo3—Mo1i | 178.56 (6) | Mo2i—Mo1—Cl3—Mo3i | 72.37 (5) |
Cl4—Mo1—Mo3—Mo1i | 123.65 (5) | Cl6—Mo3—Cl4—Mo2 | −142.73 (5) |
Cl3—Mo1—Mo3—Mo1i | −53.82 (5) | Cl2—Mo3—Cl4—Mo2 | 123.67 (5) |
Cl2—Mo1—Mo3—Mo1i | −123.36 (5) | Cl1i—Mo3—Cl4—Mo2 | 39.5 (6) |
Cl1—Mo1—Mo3—Mo1i | 53.18 (5) | Cl3i—Mo3—Cl4—Mo2 | −51.49 (5) |
Mo3i—Mo1—Mo3—Mo1i | 0.0 | Mo1i—Mo3—Cl4—Mo2 | 1.41 (3) |
Mo2—Mo1—Mo3—Mo1i | 54.84 (4) | Mo1—Mo3—Cl4—Mo2 | 72.04 (7) |
Mo2i—Mo1—Mo3—Mo1i | −55.00 (4) | Mo2i—Mo3—Cl4—Mo2 | 70.70 (7) |
Cl7—Mo1—Mo3—Mo2i | −126.45 (6) | Cl6—Mo3—Cl4—Mo1 | 145.23 (5) |
Cl4—Mo1—Mo3—Mo2i | 178.65 (4) | Cl2—Mo3—Cl4—Mo1 | 51.63 (5) |
Cl3—Mo1—Mo3—Mo2i | 1.17 (4) | Cl1i—Mo3—Cl4—Mo1 | −32.6 (6) |
Cl2—Mo1—Mo3—Mo2i | −68.36 (6) | Cl3i—Mo3—Cl4—Mo1 | −123.53 (6) |
Cl1—Mo1—Mo3—Mo2i | 108.18 (6) | Mo1i—Mo3—Cl4—Mo1 | −70.63 (7) |
Mo3i—Mo1—Mo3—Mo2i | 55.00 (4) | Mo2i—Mo3—Cl4—Mo1 | −1.34 (4) |
Mo2—Mo1—Mo3—Mo2i | 109.84 (5) | Mo2—Mo3—Cl4—Mo1 | −72.04 (7) |
Cl7—Mo1—Mo3—Mo2 | 123.72 (7) | Cl5—Mo2—Cl4—Mo3 | 144.61 (5) |
Cl4—Mo1—Mo3—Mo2 | 68.81 (6) | Cl2i—Mo2—Cl4—Mo3 | −32.4 (5) |
Cl3—Mo1—Mo3—Mo2 | −108.67 (6) | Cl3i—Mo2—Cl4—Mo3 | 51.95 (5) |
Cl2—Mo1—Mo3—Mo2 | −178.20 (3) | Cl1—Mo2—Cl4—Mo3 | −123.80 (6) |
Cl1—Mo1—Mo3—Mo2 | −1.66 (3) | Mo3i—Mo2—Cl4—Mo3 | −70.05 (6) |
Mo3i—Mo1—Mo3—Mo2 | −54.84 (4) | Mo1—Mo2—Cl4—Mo3 | −71.86 (6) |
Mo2i—Mo1—Mo3—Mo2 | −109.84 (5) | Mo1i—Mo2—Cl4—Mo3 | −1.40 (3) |
Cl5—Mo2—Mo3—Cl6 | 1.59 (7) | Cl5—Mo2—Cl4—Mo1 | −143.54 (5) |
Cl2i—Mo2—Mo3—Cl6 | −126.41 (5) | Cl2i—Mo2—Cl4—Mo1 | 39.4 (5) |
Cl3i—Mo2—Mo3—Cl6 | −55.93 (6) | Cl3i—Mo2—Cl4—Mo1 | 123.81 (5) |
Cl1—Mo2—Mo3—Cl6 | 127.32 (6) | Cl1—Mo2—Cl4—Mo1 | −51.94 (5) |
Cl4—Mo2—Mo3—Cl6 | 56.42 (5) | Mo3i—Mo2—Cl4—Mo1 | 1.81 (3) |
Mo3i—Mo2—Mo3—Cl6 | −179.65 (5) | Mo1i—Mo2—Cl4—Mo1 | 70.46 (6) |
Mo1—Mo2—Mo3—Cl6 | 125.64 (5) | Mo3—Mo2—Cl4—Mo1 | 71.86 (6) |
Mo1i—Mo2—Mo3—Cl6 | −125.02 (5) | Cl7—Mo1—Cl4—Mo3 | −144.67 (5) |
Cl5—Mo2—Mo3—Cl4 | −54.83 (6) | Cl3—Mo1—Cl4—Mo3 | 29.9 (6) |
Cl2i—Mo2—Mo3—Cl4 | 177.17 (5) | Cl2—Mo1—Cl4—Mo3 | −51.43 (4) |
Cl3i—Mo2—Mo3—Cl4 | −112.36 (6) | Cl1—Mo1—Cl4—Mo3 | 123.78 (4) |
Cl1—Mo2—Mo3—Cl4 | 70.90 (6) | Mo3i—Mo1—Cl4—Mo3 | 70.73 (6) |
Mo3i—Mo2—Mo3—Cl4 | 123.93 (4) | Mo2—Mo1—Cl4—Mo3 | 72.54 (5) |
Mo1—Mo2—Mo3—Cl4 | 69.22 (5) | Mo2i—Mo1—Cl4—Mo3 | 1.33 (3) |
Mo1i—Mo2—Mo3—Cl4 | 178.56 (3) | Cl7—Mo1—Cl4—Mo2 | 142.79 (5) |
Cl5—Mo2—Mo3—Cl2 | −125.79 (6) | Cl3—Mo1—Cl4—Mo2 | −42.7 (6) |
Cl2i—Mo2—Mo3—Cl2 | 106.21 (6) | Cl2—Mo1—Cl4—Mo2 | −123.97 (4) |
Cl3i—Mo2—Mo3—Cl2 | 176.68 (4) | Cl1—Mo1—Cl4—Mo2 | 51.24 (4) |
Cl1—Mo2—Mo3—Cl2 | −0.06 (5) | Mo3i—Mo1—Cl4—Mo2 | −1.81 (3) |
Cl4—Mo2—Mo3—Cl2 | −70.96 (6) | Mo3—Mo1—Cl4—Mo2 | −72.54 (5) |
Mo3i—Mo2—Mo3—Cl2 | 52.97 (4) | Mo2i—Mo1—Cl4—Mo2 | −71.21 (6) |
Mo1—Mo2—Mo3—Cl2 | −1.74 (3) | C4—C2—C3—C5 | −2.0 (8) |
Mo1i—Mo2—Mo3—Cl2 | 107.60 (5) | C4—C2—C3—Cl8 | 177.4 (4) |
Cl5—Mo2—Mo3—Cl1i | 128.13 (6) | C3—C2—C4—C1 | 1.6 (8) |
Cl2i—Mo2—Mo3—Cl1i | 0.13 (5) | N1—C1—C4—C2 | 179.4 (5) |
Cl3i—Mo2—Mo3—Cl1i | 70.61 (6) | N2—C1—C4—C2 | −0.4 (8) |
Cl1—Mo2—Mo3—Cl1i | −106.14 (6) | C2—C3—C5—N2 | 1.3 (8) |
Cl4—Mo2—Mo3—Cl1i | −177.04 (5) | Cl8—C3—C5—N2 | −178.1 (4) |
Mo3i—Mo2—Mo3—Cl1i | −53.11 (3) | N1—C1—N2—C5 | 179.9 (5) |
Mo1—Mo2—Mo3—Cl1i | −107.82 (5) | C4—C1—N2—C5 | −0.3 (8) |
Mo1i—Mo2—Mo3—Cl1i | 1.52 (3) | C3—C5—N2—C1 | −0.2 (8) |
Symmetry code: (i) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H2···Cl5ii | 0.89 | 2.75 | 3.472 (5) | 140 |
N1—H3···Cl6iii | 0.89 | 2.61 | 3.359 (5) | 143 |
N1—H1···Cl7iv | 0.89 | 2.39 | 3.274 (5) | 171 |
Symmetry codes: (ii) x+1, y, z−1; (iii) −x+1, −y, −z+1; (iv) x+1, −y+1/2, z−1/2. |
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