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The common structural feature of the four title IrIII compounds is the octa­hedral coordination of the IrIII atom by a PCP pincer complex, a C atom of a (eth­oxy­oxoethanyl­idene)methane group and two variable ligands X (H, CH2CO2Et, Cl) and Y (Cl, CO).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989018017024/wm5471sup1.cif
Contains datablocks global, 4, 5, 6, 7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989018017024/wm54714sup6.hkl
Contains datablock 4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989018017024/wm54715sup7.hkl
Contains datablock 5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989018017024/wm54716sup8.hkl
Contains datablock 6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989018017024/wm54717sup9.hkl
Contains datablock 7

CCDC references: 1873392; 1873391; 1873390; 1873389

Key indicators

  • Single-crystal X-ray study
  • T = 233 K
  • Mean [sigma](C-C) = 0.010 Å
  • Mean [sigma](C-C) = 0.012 Å
  • Mean [sigma](C-C) = 0.007 Å
  • Mean [sigma](C-C) = 0.006 Å
  • H-atom completeness 91%
  • Disorder in main residue
  • R factor = 0.040
  • wR factor = 0.112
  • Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Datablock: 4


Alert level A PLAT214_ALERT_2_A Atom C12 (Anion/Solvent) ADP max/min Ratio 9.0 oblate
Author Response: disorder of solvents see: _refine_special_details
PLAT260_ALERT_2_A Large Average Ueq of Residue Including       Cl7      0.203 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules CH2Cl2 and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_A Large Average Ueq of Residue Including       Cl9      0.211 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules CH2Cl2 and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details

Alert level B PLAT260_ALERT_2_B Large Average Ueq of Residue Including Cl3 0.196 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules CH2Cl2 and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details

Alert level C PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ Please Check PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by .. 22.06 Check PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........ Please Check PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.13 Do ! PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... Please Check PLAT220_ALERT_2_C Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 4.6 Ratio PLAT222_ALERT_3_C Non-Solv. Resd 1 H Uiso(max)/Uiso(min) Range 5.0 Ratio PLAT234_ALERT_4_C Large Hirshfeld Difference C103 --C104 . 0.16 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference C109 --C110 . 0.21 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference C110 --C111 . 0.16 Ang. PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C102 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C103 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C109 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C411 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C101 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C104 Check PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C11 Check PLAT260_ALERT_2_C Large Average Ueq of Residue Including Cl5 0.115 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules CH2Cl2 and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including       Cl2      0.108 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules CH2Cl2 and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT336_ALERT_2_C Long Bond Distance for ..... C11      -Cl7A           2.060 Ang.
PLAT336_ALERT_2_C Long Bond Distance for ..... C12      -Cl9            2.030 Ang.
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0099 Ang.
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.886 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.595         28 Report
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  1.04A   From O2              0.93 eA-3

Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C57.75 H56.5 Cl7.5 Ir1 O2 P4 Atom count from the _atom_site data: C57.75 H51 Cl7.5 Ir1 O2 P4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C57.75 H56.50 Cl7.50 Ir O2 P4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 231.00 231.00 0.00 H 226.00 204.00 22.00 Cl 30.00 30.00 0.00 Ir 4.00 4.00 0.00 O 8.00 8.00 0.00 P 16.00 16.00 0.00 PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 4 Note PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 0.25 Check PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 10.28 Why ? PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 Note PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 2 Report PLAT300_ALERT_4_G Atom Site Occupancy of Cl7 Constrained at 0.7 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl8 Constrained at 0.7 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl7A Constrained at 0.3 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl8A Constrained at 0.3 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl3 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl4 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C9 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl9 Constrained at 0.25 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl10 Constrained at 0.25 Check PLAT300_ALERT_4_G Atom Site Occupancy of C12 Constrained at 0.25 Check PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 2 ) 67% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 3 ) 100% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 5 ) 100% Note PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 3 1.50 Check PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 5 0.75 Check PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C4 Check PLAT344_ALERT_2_G Unusual sp? Angle Range in Solvent/Ion for C10 Check PLAT367_ALERT_2_G Long? C(sp?)-C(sp?) Bond C1 - C4 . 1.52 Ang. PLAT432_ALERT_2_G Short Inter X...Y Contact Cl9 ..C12 2.23 Ang. 2-x,-y,-z = 3_755 Check PLAT432_ALERT_2_G Short Inter X...Y Contact Cl9 ..C11 3.20 Ang. x,y,z = 1_555 Check PLAT432_ALERT_2_G Short Inter X...Y Contact Cl10 ..C12 3.15 Ang. 2-x,-y,-z = 3_755 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C12 ..C12 1.79 Ang. 2-x,-y,-z = 3_755 Check PLAT773_ALERT_2_G Check long C-C Bond in CIF: C12 --C12 1.79 Ang. PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note C Cl2 PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 2 Note PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 61% Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 1 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 25 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 1 Info
3 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 25 ALERT level C = Check. Ensure it is not caused by an omission or oversight 38 ALERT level G = General information/check it is not something unexpected 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 29 ALERT type 2 Indicator that the structure model may be wrong or deficient 9 ALERT type 3 Indicator that the structure quality may be low 22 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Datablock: 5
Alert level A THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5371
Author Response: low diffraction because of small crystal size see: _refine_special_details
PLAT023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.44 Degree
Author Response: low diffraction because of small crystal size see: _refine_special_details
PLAT430_ALERT_2_A Short Inter D...A Contact  O6       ..O6       .       1.60 Ang.
                                               -1-x,1-y,2-z  =      2_467 Check
Author Response: disorder of solvents see: _refine_special_details
PLAT430_ALERT_2_A Short Inter D...A Contact  O6       ..O7       .       1.86 Ang.
                                               -1-x,1-y,2-z  =      2_467 Check
Author Response: disorder of solvents see: _refine_special_details

Alert level B PLAT216_ALERT_3_B Disordered C13 (An/Solv) ADP max/min Ratio 8.6 Note
Author Response: disorder of solvents see: _refine_special_details
PLAT260_ALERT_2_B Large Average Ueq of Residue Including        O5      0.179 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_B Large Average Ueq of Residue Including        O6      0.191 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT410_ALERT_2_B Short Intra H...H Contact  H3A      ..H402     .       1.86 Ang.
                                                      x,y,z  =      1_555 Check
Author Response: disorder,low diffraction because of small crystal size see: _refine_special_details
PLAT430_ALERT_2_B Short Inter D...A Contact  O6       ..O7       .       2.61 Ang.
                                                      x,y,z  =      1_555 Check
Author Response: disorder of solvents see: _refine_special_details

Alert level C PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ Please Check PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by .. 10.02 Check PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........ Please Check PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.12 Do ! PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... Please Check PLAT222_ALERT_3_C Non-Solv. Resd 1 H Uiso(max)/Uiso(min) Range 10.0 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ir1 --P4 . 5.5 s.u. PLAT245_ALERT_2_C U(iso) H4 Smaller than U(eq) C4 by 0.028 Ang   2 PLAT260_ALERT_2_C Large Average Ueq of Residue Including Cl2 0.143 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including        O7      0.113 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........         O5 Check
PLAT309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........         O6 Check
PLAT330_ALERT_2_C Large Aver Phenyl C-C Dist C41A      -C46A     .       1.41 Ang.
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01228 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A      ..CL2      .       2.91 Ang.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         58 Ang   3
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1 Note
              C59 H57 Cl Ir O4 P4
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.804 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.537         24 Report

Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C60 H62 Cl2 Ir1 O5.5 P4 Atom count from the _atom_site data: C60 H57 Cl2 Ir1 O5.5 P4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C60 H62 Cl2 Ir O5.50 P4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 120.00 120.00 0.00 H 124.00 114.00 10.00 Cl 4.00 4.00 0.00 Ir 2.00 2.00 0.00 O 11.00 11.00 0.00 P 8.00 8.00 0.00 PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 2 Note PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 0.50 Check PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 6.95 Why ? PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.002 Degree PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 Note PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 1 Report PLAT300_ALERT_4_G Atom Site Occupancy of C41A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C42A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C43A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C44A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C45A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C46A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C401 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C402 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C403 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C404 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C405 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C406 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H42A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H43A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H44A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H45A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H46A Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H402 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H403 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H404 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H405 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of H406 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of O5 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C12 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of O6 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of C13 Constrained at 0.5 Check PLAT300_ALERT_4_G Atom Site Occupancy of O7 Constrained at 0.5 Check PLAT301_ALERT_3_G Main Residue Disorder ..............(Resd 1 ) 9% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 2 ) 100% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 3 ) 100% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 5 ) 100% Note PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 5 0.50 Check PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) ..... O7 Check PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C4 Check PLAT367_ALERT_2_G Long? C(sp?)-C(sp?) Bond C1 - C4 . 1.51 Ang. PLAT431_ALERT_2_G Short Inter HL..A Contact Cl2 ..O5 . 2.94 Ang. x,y,z = 1_555 Check PLAT432_ALERT_2_G Short Inter X...Y Contact O5 ..C13 2.58 Ang. -1-x,1-y,2-z = 2_467 Check PLAT432_ALERT_2_G Short Inter X...Y Contact O6 ..C13 2.70 Ang. -1-x,1-y,2-z = 2_467 Check PLAT432_ALERT_2_G Short Inter X...Y Contact O7 ..C13 0.97 Ang. -1-x,1-y,2-z = 2_467 Check PLAT432_ALERT_2_G Short Inter X...Y Contact O7 ..C12 2.82 Ang. x,y,z = 1_555 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C12 ..C13 2.08 Ang. -1-x,1-y,2-z = 2_467 Check PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note C O PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 3 Note C O PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 4 Note Cl PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 5 Note O PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 1 Note PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 69% Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 4 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 15 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 1 Info
4 ALERT level A = Most likely a serious problem - resolve or explain 5 ALERT level B = A potentially serious problem, consider carefully 19 ALERT level C = Check. Ensure it is not caused by an omission or oversight 59 ALERT level G = General information/check it is not something unexpected 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 28 ALERT type 2 Indicator that the structure model may be wrong or deficient 12 ALERT type 3 Indicator that the structure quality may be low 39 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Datablock: 6
Alert level B PLAT260_ALERT_2_B Large Average Ueq of Residue Including O5 0.171 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......         O4 Check
Author Response: solvent without hydrogens see: _refine_special_details
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check
Author Response: solvent without hydrogens see: _refine_special_details
PLAT430_ALERT_2_B Short Inter D...A Contact  O3       ..O4       .       2.74 Ang.
                                                      x,y,z  =      1_555 Check
Author Response: solvent without hydrogens see: _refine_special_details

Alert level C PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ Please Check PLAT043_ALERT_1_C Calculated and Reported Mol. Weight Differ by .. 8.04 Check PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........ Please Check PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... Please Check PLAT220_ALERT_2_C Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 3.4 Ratio PLAT222_ALERT_3_C Non-Solv. Resd 1 H Uiso(max)/Uiso(min) Range 6.0 Ratio PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C111 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C403 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C401 Check PLAT260_ALERT_2_C Large Average Ueq of Residue Including O3 0.140 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including       Cl3      0.088 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including        O4      0.127 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........         O3 Check
PLAT410_ALERT_2_C Short Intra H...H Contact  H2B      ..H112     .       1.97 Ang.
                                                      x,y,z  =      1_555 Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H206     ..CL3      .       2.87 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H312     ..CL3      .       2.84 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H406     ..CL3      .       2.88 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H412     ..CL3      .       2.95 Ang.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         46 Ang   3
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.595         19 Report
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  1.03A   From O5              0.44 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C56 H58 Cl3 Ir1 O5 P4 Atom count from the _atom_site data: C56 H50 Cl3 Ir1 O5 P4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C56 H58 Cl3 Ir O5 P4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 112.00 112.00 0.00 H 116.00 100.00 16.00 Cl 6.00 6.00 0.00 Ir 2.00 2.00 0.00 O 10.00 10.00 0.00 P 8.00 8.00 0.00 PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 2 Note PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.001 Degree PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 Note PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 1 Report PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C4 Check PLAT344_ALERT_2_G Unusual sp? Angle Range in Solvent/Ion for C8 Check PLAT367_ALERT_2_G Long? C(sp?)-C(sp?) Bond C1 - C4 . 1.51 Ang. PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note C O PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 1 Note PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 66% Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 3 Note PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 1 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 15 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 4 ALERT level B = A potentially serious problem, consider carefully 22 ALERT level C = Check. Ensure it is not caused by an omission or oversight 16 ALERT level G = General information/check it is not something unexpected 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 22 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Datablock: 7
Alert level A PLAT260_ALERT_2_A Large Average Ueq of Residue Including Cl5A 0.240 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details

Alert level B PLAT057_ALERT_3_B Correction for Absorption Required RT(exp) ... 1.23 Do !
Author Response: correction in a multiscan-like manner, see: _exptl_special_details

Alert level C PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ Please Check PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........ Please Check PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... Please Check PLAT220_ALERT_2_C Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 3.9 Ratio PLAT222_ALERT_3_C Non-Solv. Resd 1 H Uiso(max)/Uiso(min) Range 5.0 Ratio PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C211 Check PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C13 Check PLAT245_ALERT_2_C U(iso) H6OB Smaller than U(eq) O6 by 0.040 Ang   2 PLAT260_ALERT_2_C Large Average Ueq of Residue Including Cl3 0.120 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including       Cl5      0.130 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including        O6      0.118 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT260_ALERT_2_C Large Average Ueq of Residue Including        O7      0.141 Check
Author Response: disorder of solvents,these atoms are part of the solvent molecules and show strong vibrations, which were underlined by a high temperature factor. see: _refine_special_details
PLAT410_ALERT_2_C Short Intra H...H Contact  H3A      ..H412     .       1.98 Ang.
                                                      x,y,z  =      1_555 Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H108     ..O2       .       2.61 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H412     ..CL1      .       2.97 Ang.
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         10 Report
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C62 H64 Cl6 Ir1 O6.5 P4 Atom count from the _atom_site data: C62 H63 Cl6 Ir1 O6.5 P4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C62 H64 Cl6 Ir O6.50 P4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 124.00 124.00 0.00 H 128.00 126.00 2.00 Cl 12.00 12.00 0.00 Ir 2.00 2.00 0.00 O 13.00 13.00 0.00 P 8.00 8.00 0.00 PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 5 Note PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 0.50 Check PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 5.25 Why ? PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.001 Degree PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct. 1 Note PLAT171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records 1 Report PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 2 Report PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Ir1 --C12 . 5.4 s.u. PLAT300_ALERT_4_G Atom Site Occupancy of Cl5 Constrained at 0.65 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl6 Constrained at 0.65 Check PLAT300_ALERT_4_G Atom Site Occupancy of C14 Constrained at 0.65 Check PLAT300_ALERT_4_G Atom Site Occupancy of H14A Constrained at 0.65 Check PLAT300_ALERT_4_G Atom Site Occupancy of H14B Constrained at 0.65 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl5A Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of Cl6A Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of C14A Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of H14C Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of H14D Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of O7 Constrained at 0.5 Check PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 3 ) 100% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 4 ) 100% Note PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd 8 ) 100% Note PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 3 3.25 Check PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 4 1.75 Check PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 8 0.50 Check PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) ..... O7 Check PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C4 Check PLAT367_ALERT_2_G Long? C(sp?)-C(sp?) Bond C1 - C4 . 1.51 Ang. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 2 Note PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 3 Note C H2 Cl2 PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 4 Note C H2 Cl2 PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 5 Note Cl PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 8 Note O PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 3 Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 4 Note PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 3 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 5 Note
1 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 17 ALERT level C = Check. Ensure it is not caused by an omission or oversight 40 ALERT level G = General information/check it is not something unexpected 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 18 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 28 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level A PUBL024_ALERT_1_A The number of authors is greater than 5. Please specify the role of each of the co-authors for your paper.
1 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing

Computing details top

For all structures, data collection: COLLECT (Nonius, 1999); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010) and CHEMDRAW (Cambridge Soft, 2001).

(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}(ethoxyoxoethanylidene)methane-κ4P,C,C',P')chloridohydridoiridium(III) chloride methylene chloride 2.75-solvate (4) top
Crystal data top
[IrClH(C55H50O2P4)]Cl·2.75CH2Cl2F(000) = 2734
Mr = 1364.48Dx = 1.448 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 12.4425 (2) ÅCell parameters from 104186 reflections
b = 22.4020 (3) Åθ = 1.0–25.3°
c = 22.5393 (3) ŵ = 2.59 mm1
β = 94.826 (1)°T = 233 K
V = 6260.26 (16) Å3Prism, colorless
Z = 40.11 × 0.08 × 0.05 mm
Data collection top
Nonius KappaCCD
diffractometer
8888 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.045
Graphite monochromatorθmax = 25.0°, θmin = 1.8°
phi– and ω–scansh = 1414
39699 measured reflectionsk = 2626
11006 independent reflectionsl = 2626
Refinement top
Refinement on F22 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.040H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0606P)2 + 10.2768P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
11006 reflectionsΔρmax = 1.03 e Å3
711 parametersΔρmin = 0.86 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Hyrogen atoms at Ir1 and C4 were localized and refined with bond restraints: 96 pm at C4 and 160 pm at Ir1, respectively. There are four solvent molecules into the asymmetric unit, which are partial disordered (C9 occupational disorder with factor 0.5, C11 positional disorder of chlorine atoms wiht ratio 7:3 and C12 occupational disorder with factor 0.25). Hydrogen atoms at solvent were omitted.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ir10.49207 (2)0.11833 (2)0.20622 (2)0.03228 (8)
H10.484 (4)0.1906 (9)0.209 (2)0.067 (18)*
P10.67637 (10)0.11984 (5)0.22113 (6)0.0370 (3)
P20.62189 (10)0.01107 (5)0.22879 (6)0.0365 (3)
P30.36683 (10)0.01314 (5)0.21373 (5)0.0326 (3)
P40.30844 (10)0.11776 (5)0.19399 (6)0.0322 (3)
Cl10.52098 (11)0.12563 (6)0.09975 (6)0.0461 (3)
Cl20.98655 (13)0.01266 (9)0.20289 (13)0.1081 (9)
O10.3419 (3)0.04012 (18)0.33389 (18)0.0627 (11)
O20.4452 (4)0.11608 (16)0.36960 (17)0.0579 (11)
C10.4926 (4)0.02169 (19)0.2370 (2)0.0323 (10)
C20.7115 (4)0.0439 (2)0.1997 (2)0.0424 (12)
H2A0.70700.04100.15620.051*
H2B0.78600.03520.21480.051*
C30.2600 (4)0.0420 (2)0.2099 (2)0.0396 (11)
H3A0.22700.04250.24790.048*
H3B0.20420.03040.17880.048*
C40.4981 (4)0.0697 (2)0.2846 (2)0.0360 (11)
H40.571 (2)0.068 (2)0.3031 (19)0.036 (13)*
C50.4185 (5)0.0725 (2)0.3304 (2)0.0443 (12)
C70.3729 (7)0.1253 (3)0.4152 (3)0.076 (2)
H7A0.36760.08900.43920.091*
H7B0.30070.13570.39750.091*
C80.4203 (8)0.1761 (4)0.4533 (4)0.118 (3)
H8A0.37440.18420.48510.177*
H8B0.49180.16500.47040.177*
H8C0.42520.21150.42890.177*
C1010.7549 (4)0.1701 (2)0.1780 (2)0.0463 (13)
C1020.8362 (7)0.1526 (4)0.1455 (5)0.115 (4)
H1020.85380.11190.14380.138*
C1030.8944 (8)0.1940 (5)0.1145 (6)0.149 (5)
H1030.94910.18110.09110.179*
C1040.8713 (6)0.2521 (4)0.1183 (4)0.095 (3)
H1040.91050.28000.09780.114*
C1050.7917 (8)0.2712 (3)0.1516 (4)0.093 (3)
H1050.77760.31230.15490.112*
C1060.7311 (7)0.2298 (3)0.1808 (3)0.080 (2)
H1060.67400.24270.20240.096*
C1070.7388 (5)0.1311 (2)0.2962 (3)0.0514 (14)
C1080.8387 (6)0.1063 (3)0.3146 (3)0.073 (2)
H1080.87620.08270.28860.088*
C1090.8822 (8)0.1176 (4)0.3736 (5)0.112 (4)
H1090.94900.10090.38740.134*
C1100.8274 (11)0.1528 (5)0.4107 (4)0.115 (4)
H1100.85760.15990.44970.138*
C1110.7302 (8)0.1776 (4)0.3923 (3)0.091 (3)
H1110.69380.20200.41810.110*
C1120.6863 (6)0.1664 (3)0.3353 (3)0.0651 (17)
H1120.61900.18310.32250.078*
C2010.6228 (4)0.0736 (2)0.1787 (2)0.0409 (12)
C2020.6137 (5)0.0644 (3)0.1167 (2)0.0499 (14)
H2020.60520.02550.10140.060*
C2030.6174 (6)0.1124 (3)0.0783 (3)0.0681 (18)
H2030.61040.10630.03690.082*
C2040.6316 (5)0.1700 (3)0.1014 (3)0.0673 (18)
H2040.63550.20270.07550.081*
C2050.6399 (5)0.1793 (3)0.1620 (3)0.0648 (17)
H2050.64780.21830.17710.078*
C2060.6368 (4)0.1317 (2)0.2010 (3)0.0524 (14)
H2060.64410.13830.24230.063*
C2070.6860 (5)0.0357 (2)0.2990 (3)0.0491 (14)
C2080.7957 (5)0.0481 (3)0.3027 (3)0.0682 (18)
H2080.83470.04410.26900.082*
C2090.8477 (8)0.0666 (4)0.3568 (5)0.100 (3)
H2090.92190.07520.35920.120*
C2100.7930 (10)0.0726 (4)0.4060 (4)0.106 (4)
H2100.82990.08420.44220.127*
C2110.6813 (9)0.0614 (3)0.4032 (3)0.096 (3)
H2110.64350.06640.43730.116*
C2120.6259 (6)0.0425 (3)0.3485 (3)0.0657 (18)
H2120.55140.03470.34570.079*
C3010.3231 (4)0.0735 (2)0.2590 (2)0.0384 (11)
C3020.2144 (5)0.0820 (3)0.2652 (3)0.0572 (15)
H3020.16370.05440.24860.069*
C3030.1802 (6)0.1309 (3)0.2959 (3)0.077 (2)
H3030.10620.13660.29960.092*
C3040.2540 (7)0.1712 (3)0.3209 (3)0.078 (2)
H3040.23030.20400.34230.094*
C3050.3607 (6)0.1639 (3)0.3150 (3)0.0711 (19)
H3050.41100.19170.33190.085*
C3060.3953 (5)0.1149 (2)0.2835 (3)0.0554 (15)
H3060.46920.11000.27910.067*
C3070.3642 (4)0.0446 (2)0.1398 (2)0.0356 (11)
C3080.3715 (5)0.0068 (2)0.0913 (2)0.0494 (13)
H3080.38520.03410.09730.059*
C3090.3585 (6)0.0297 (3)0.0343 (3)0.0690 (18)
H3090.36340.00420.00150.083*
C3100.3382 (6)0.0895 (3)0.0250 (3)0.0686 (18)
H3100.32910.10480.01400.082*
C3110.3314 (6)0.1269 (3)0.0729 (3)0.0625 (17)
H3110.31790.16780.06670.075*
C3120.3444 (5)0.1046 (2)0.1300 (2)0.0472 (13)
H3120.33970.13050.16260.057*
C4010.2343 (4)0.1642 (2)0.2433 (2)0.0402 (11)
C4020.2883 (5)0.2051 (2)0.2807 (2)0.0483 (13)
H4020.36370.20860.28170.058*
C4030.2304 (5)0.2412 (3)0.3171 (3)0.0607 (16)
H4030.26710.26900.34260.073*
C4040.1209 (5)0.2365 (3)0.3161 (3)0.0636 (17)
H4040.08270.26060.34120.076*
C4050.0667 (5)0.1966 (3)0.2782 (4)0.078 (2)
H4050.00880.19360.27720.094*
C4060.1231 (5)0.1603 (3)0.2410 (3)0.0690 (19)
H4060.08580.13340.21470.083*
C4070.2442 (4)0.1381 (2)0.1209 (2)0.0421 (12)
C4080.2823 (5)0.1899 (2)0.0957 (2)0.0507 (14)
H4080.34160.21000.11500.061*
C4090.2344 (6)0.2122 (3)0.0426 (3)0.0676 (18)
H4090.25970.24780.02680.081*
C4100.1496 (6)0.1820 (4)0.0132 (3)0.080 (2)
H4100.11620.19710.02270.096*
C4110.1144 (7)0.1301 (4)0.0363 (4)0.093 (3)
H4110.05870.10870.01510.111*
C4120.1591 (6)0.1078 (3)0.0910 (3)0.0708 (19)
H4120.13170.07280.10720.085*
C90.250 (3)0.0515 (13)0.4305 (9)0.223 (19)0.5
Cl30.3575 (9)0.0543 (4)0.4754 (3)0.201 (4)0.5
Cl40.1305 (7)0.0182 (4)0.4559 (3)0.167 (3)0.5
C100.5629 (8)0.2613 (4)0.0386 (4)0.112 (3)
Cl50.4809 (2)0.31145 (11)0.07504 (11)0.1086 (7)
Cl60.6123 (3)0.29238 (12)0.02166 (12)0.1243 (9)
C110.9453 (10)0.1288 (5)0.1519 (7)0.139 (4)
Cl70.9402 (6)0.1902 (3)0.1966 (6)0.197 (4)0.7
Cl81.0617 (3)0.1332 (3)0.1087 (2)0.1348 (16)0.7
Cl7A0.9153 (19)0.1694 (9)0.231 (2)0.31 (2)0.3
Cl8A1.0197 (18)0.1825 (9)0.1312 (12)0.239 (10)0.3
C120.951 (5)0.0067 (16)0.026 (3)0.16 (2)0.25
Cl91.0704 (12)0.0453 (9)0.0654 (12)0.238 (11)0.25
Cl100.8652 (16)0.0098 (9)0.0607 (12)0.234 (11)0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.03166 (12)0.02717 (12)0.03855 (12)0.00054 (7)0.00623 (8)0.00117 (8)
P10.0320 (7)0.0297 (7)0.0491 (8)0.0032 (5)0.0014 (6)0.0026 (5)
P20.0328 (7)0.0302 (6)0.0466 (7)0.0015 (5)0.0025 (5)0.0026 (6)
P30.0327 (6)0.0274 (6)0.0387 (7)0.0006 (5)0.0085 (5)0.0005 (5)
P40.0309 (6)0.0272 (6)0.0392 (7)0.0035 (5)0.0069 (5)0.0008 (5)
Cl10.0470 (7)0.0514 (8)0.0414 (7)0.0001 (6)0.0130 (6)0.0066 (6)
Cl20.0366 (9)0.0594 (11)0.229 (3)0.0004 (7)0.0143 (12)0.0035 (13)
O10.071 (3)0.059 (3)0.063 (3)0.014 (2)0.029 (2)0.008 (2)
O20.082 (3)0.051 (2)0.043 (2)0.0040 (19)0.017 (2)0.0143 (18)
C10.036 (3)0.026 (2)0.035 (3)0.0005 (19)0.007 (2)0.002 (2)
C20.030 (3)0.034 (3)0.064 (3)0.000 (2)0.007 (2)0.003 (2)
C30.032 (3)0.035 (3)0.052 (3)0.001 (2)0.009 (2)0.001 (2)
C40.037 (3)0.029 (3)0.042 (3)0.000 (2)0.004 (2)0.000 (2)
C50.054 (3)0.039 (3)0.041 (3)0.002 (3)0.011 (2)0.002 (2)
C70.105 (6)0.079 (5)0.049 (4)0.004 (4)0.034 (4)0.014 (3)
C80.153 (9)0.120 (7)0.087 (6)0.003 (6)0.036 (6)0.058 (6)
C1010.036 (3)0.045 (3)0.056 (3)0.006 (2)0.002 (2)0.010 (3)
C1020.087 (6)0.064 (5)0.206 (10)0.008 (4)0.085 (6)0.036 (6)
C1030.112 (8)0.098 (7)0.254 (14)0.014 (6)0.117 (9)0.062 (8)
C1040.063 (5)0.103 (7)0.117 (7)0.036 (5)0.000 (5)0.047 (6)
C1050.128 (7)0.047 (4)0.106 (6)0.020 (4)0.020 (6)0.022 (4)
C1060.112 (6)0.045 (4)0.089 (5)0.006 (4)0.039 (5)0.007 (4)
C1070.050 (3)0.043 (3)0.059 (4)0.015 (3)0.011 (3)0.008 (3)
C1080.063 (4)0.069 (4)0.084 (5)0.009 (3)0.025 (4)0.009 (4)
C1090.095 (7)0.098 (7)0.129 (9)0.027 (5)0.072 (7)0.031 (6)
C1100.149 (10)0.114 (8)0.074 (6)0.053 (7)0.027 (6)0.005 (6)
C1110.115 (7)0.091 (6)0.066 (5)0.045 (5)0.004 (5)0.007 (4)
C1120.076 (4)0.057 (4)0.062 (4)0.022 (3)0.002 (3)0.009 (3)
C2010.032 (3)0.033 (3)0.059 (3)0.001 (2)0.009 (2)0.006 (2)
C2020.057 (4)0.043 (3)0.052 (3)0.001 (3)0.018 (3)0.001 (3)
C2030.071 (4)0.072 (5)0.064 (4)0.007 (3)0.024 (3)0.017 (3)
C2040.066 (4)0.051 (4)0.088 (5)0.004 (3)0.024 (4)0.028 (4)
C2050.058 (4)0.039 (3)0.099 (5)0.003 (3)0.015 (4)0.009 (3)
C2060.041 (3)0.039 (3)0.077 (4)0.002 (2)0.008 (3)0.001 (3)
C2070.055 (3)0.035 (3)0.054 (3)0.002 (2)0.013 (3)0.002 (2)
C2080.055 (4)0.055 (4)0.090 (5)0.005 (3)0.020 (3)0.010 (3)
C2090.089 (6)0.074 (5)0.126 (8)0.009 (4)0.060 (6)0.015 (5)
C2100.154 (9)0.064 (5)0.086 (6)0.037 (5)0.066 (6)0.004 (5)
C2110.171 (9)0.064 (5)0.052 (4)0.025 (5)0.005 (5)0.002 (3)
C2120.092 (5)0.046 (3)0.057 (4)0.016 (3)0.006 (3)0.010 (3)
C3010.047 (3)0.035 (3)0.034 (3)0.005 (2)0.011 (2)0.002 (2)
C3020.053 (4)0.050 (3)0.071 (4)0.005 (3)0.016 (3)0.013 (3)
C3030.076 (5)0.070 (5)0.091 (5)0.016 (4)0.034 (4)0.014 (4)
C3040.102 (6)0.056 (4)0.079 (5)0.018 (4)0.028 (4)0.022 (4)
C3050.093 (5)0.047 (4)0.073 (4)0.003 (4)0.007 (4)0.017 (3)
C3060.064 (4)0.045 (3)0.059 (4)0.002 (3)0.016 (3)0.012 (3)
C3070.034 (3)0.034 (3)0.040 (3)0.002 (2)0.009 (2)0.000 (2)
C3080.068 (4)0.040 (3)0.042 (3)0.002 (3)0.015 (3)0.001 (2)
C3090.103 (5)0.060 (4)0.046 (3)0.008 (4)0.017 (3)0.003 (3)
C3100.094 (5)0.070 (4)0.044 (3)0.005 (4)0.016 (3)0.018 (3)
C3110.082 (5)0.052 (4)0.055 (4)0.014 (3)0.017 (3)0.022 (3)
C3120.058 (3)0.038 (3)0.048 (3)0.003 (2)0.015 (3)0.004 (2)
C4010.041 (3)0.034 (3)0.047 (3)0.001 (2)0.013 (2)0.002 (2)
C4020.047 (3)0.048 (3)0.050 (3)0.008 (3)0.008 (3)0.006 (3)
C4030.064 (4)0.058 (4)0.060 (4)0.013 (3)0.005 (3)0.021 (3)
C4040.072 (4)0.045 (3)0.079 (4)0.008 (3)0.035 (4)0.011 (3)
C4050.053 (4)0.061 (4)0.127 (6)0.003 (3)0.046 (4)0.031 (4)
C4060.049 (4)0.057 (4)0.104 (5)0.011 (3)0.030 (3)0.036 (4)
C4070.039 (3)0.043 (3)0.045 (3)0.010 (2)0.004 (2)0.003 (2)
C4080.056 (3)0.046 (3)0.050 (3)0.008 (3)0.003 (3)0.002 (3)
C4090.079 (5)0.062 (4)0.062 (4)0.013 (4)0.006 (4)0.010 (3)
C4100.087 (5)0.092 (6)0.059 (4)0.013 (4)0.011 (4)0.010 (4)
C4110.076 (5)0.115 (7)0.080 (5)0.014 (5)0.034 (4)0.003 (5)
C4120.062 (4)0.076 (5)0.070 (4)0.010 (3)0.021 (3)0.004 (3)
C90.41 (4)0.20 (2)0.070 (12)0.24 (3)0.11 (2)0.077 (14)
Cl30.324 (12)0.154 (6)0.121 (5)0.103 (7)0.006 (6)0.008 (5)
Cl40.197 (7)0.205 (7)0.099 (4)0.039 (6)0.008 (4)0.037 (4)
C100.142 (8)0.072 (5)0.126 (8)0.001 (5)0.032 (6)0.029 (5)
Cl50.1132 (17)0.1046 (17)0.1117 (17)0.0339 (13)0.0310 (14)0.0231 (13)
Cl60.160 (2)0.1072 (18)0.1116 (18)0.0022 (17)0.0446 (17)0.0005 (15)
C110.101 (8)0.117 (9)0.195 (13)0.018 (7)0.007 (8)0.027 (8)
Cl70.103 (5)0.089 (4)0.393 (14)0.018 (3)0.010 (6)0.043 (6)
Cl80.088 (3)0.194 (5)0.118 (3)0.029 (3)0.020 (2)0.020 (3)
Cl7A0.128 (13)0.102 (12)0.69 (7)0.008 (9)0.05 (2)0.04 (2)
Cl8A0.201 (19)0.174 (15)0.32 (3)0.048 (14)0.098 (18)0.041 (16)
C120.22 (6)0.04 (2)0.22 (6)0.08 (3)0.03 (4)0.05 (3)
Cl90.120 (11)0.208 (18)0.39 (3)0.022 (11)0.010 (14)0.15 (2)
Cl100.159 (14)0.213 (19)0.31 (3)0.077 (14)0.088 (16)0.088 (18)
Geometric parameters (Å, º) top
Ir1—C42.072 (5)C207—C2081.390 (8)
Ir1—C12.273 (4)C207—C2121.402 (9)
Ir1—P42.2783 (12)C208—C2091.394 (10)
Ir1—P12.2897 (13)C208—H2080.9400
Ir1—Cl12.4619 (13)C209—C2101.355 (13)
Ir1—H11.62 (2)C209—H2090.9400
P1—C1071.819 (6)C210—C2111.408 (13)
P1—C1011.824 (5)C210—H2100.9400
P1—C21.833 (5)C211—C2121.426 (9)
P2—C11.791 (5)C211—H2110.9400
P2—C2071.798 (5)C212—H2120.9400
P2—C2011.800 (5)C301—C3061.374 (8)
P2—C21.820 (5)C301—C3021.384 (7)
P3—C11.788 (5)C302—C3031.380 (9)
P3—C3011.806 (5)C302—H3020.9400
P3—C3071.807 (5)C303—C3041.376 (10)
P3—C31.811 (5)C303—H3030.9400
P4—C4071.827 (5)C304—C3051.356 (10)
P4—C4011.828 (5)C304—H3040.9400
P4—C31.846 (5)C305—C3061.396 (8)
O1—C51.205 (6)C305—H3050.9400
O2—C51.341 (6)C306—H3060.9400
O2—C71.437 (7)C307—C3121.383 (7)
C1—C41.515 (6)C307—C3081.391 (7)
C2—H2A0.9800C308—C3091.380 (8)
C2—H2B0.9800C308—H3080.9400
C3—H3A0.9800C309—C3101.376 (9)
C3—H3B0.9800C309—H3090.9400
C4—C51.490 (7)C310—C3111.375 (9)
C4—H40.968 (19)C310—H3100.9400
C7—C81.516 (10)C311—C3121.378 (8)
C7—H7A0.9800C311—H3110.9400
C7—H7B0.9800C312—H3120.9400
C8—H8A0.9700C401—C4021.381 (7)
C8—H8B0.9700C401—C4061.383 (8)
C8—H8C0.9700C402—C4031.395 (8)
C101—C1021.356 (9)C402—H4020.9400
C101—C1061.371 (8)C403—C4041.364 (9)
C102—C1031.399 (11)C403—H4030.9400
C102—H1020.9400C404—C4051.375 (9)
C103—C1041.337 (13)C404—H4040.9400
C103—H1030.9400C405—C4061.397 (8)
C104—C1051.360 (12)C405—H4050.9400
C104—H1040.9400C406—H4060.9400
C105—C1061.396 (10)C407—C4121.385 (8)
C105—H1050.9400C407—C4081.392 (8)
C106—H1060.9400C408—C4091.383 (8)
C107—C1121.389 (9)C408—H4080.9400
C107—C1081.393 (9)C409—C4101.376 (10)
C108—C1091.416 (12)C409—H4090.9400
C108—H1080.9400C410—C4111.362 (11)
C109—C1101.372 (15)C410—H4100.9400
C109—H1090.9400C411—C4121.402 (10)
C110—C1111.364 (14)C411—H4110.9400
C110—H1100.9400C412—H4120.9400
C111—C1121.376 (10)C9—Cl31.61 (4)
C111—H1110.9400C9—Cl41.80 (4)
C112—H1120.9400C10—Cl61.687 (9)
C201—C2061.399 (7)C10—Cl51.766 (10)
C201—C2021.409 (8)C11—Cl8A1.61 (2)
C202—C2031.384 (8)C11—Cl71.709 (18)
C202—H2020.9400C11—Cl81.815 (15)
C203—C2041.399 (9)C11—Cl7A2.07 (4)
C203—H2030.9400Cl8—Cl92.21 (3)
C204—C2051.377 (10)C12—Cl101.37 (5)
C204—H2040.9400C12—C12i1.79 (12)
C205—C2061.384 (8)C12—Cl92.02 (7)
C205—H2050.9400C12—Cl9i2.24 (6)
C206—H2060.9400Cl9—C12i2.24 (6)
C4—Ir1—C140.49 (17)C203—C202—H202119.9
C4—Ir1—P493.68 (14)C201—C202—H202119.9
C1—Ir1—P490.52 (12)C202—C203—C204119.6 (6)
C4—Ir1—P185.34 (14)C202—C203—H203120.2
C1—Ir1—P189.54 (12)C204—C203—H203120.2
P4—Ir1—P1178.42 (5)C205—C204—C203120.4 (6)
C4—Ir1—Cl1150.26 (13)C205—C204—H204119.8
C1—Ir1—Cl1111.34 (12)C203—C204—H204119.8
P4—Ir1—Cl196.30 (4)C204—C205—C206120.6 (6)
P1—Ir1—Cl185.15 (5)C204—C205—H205119.7
C4—Ir1—H1119.7 (18)C206—C205—H205119.7
C1—Ir1—H1159.8 (18)C205—C206—C201119.9 (6)
P4—Ir1—H187.0 (18)C205—C206—H206120.0
P1—Ir1—H192.4 (18)C201—C206—H206120.0
Cl1—Ir1—H188.8 (18)C208—C207—C212121.2 (6)
C107—P1—C101101.8 (2)C208—C207—P2118.4 (5)
C107—P1—C2106.3 (3)C212—C207—P2120.5 (5)
C101—P1—C2106.4 (2)C207—C208—C209119.6 (8)
C107—P1—Ir1118.9 (2)C207—C208—H208120.2
C101—P1—Ir1120.39 (17)C209—C208—H208120.2
C2—P1—Ir1101.87 (16)C210—C209—C208121.1 (8)
C1—P2—C207111.7 (3)C210—C209—H209119.5
C1—P2—C201115.9 (2)C208—C209—H209119.5
C207—P2—C201106.7 (2)C209—C210—C211120.6 (7)
C1—P2—C2110.1 (2)C209—C210—H210119.7
C207—P2—C2106.6 (3)C211—C210—H210119.7
C201—P2—C2105.3 (2)C210—C211—C212119.6 (8)
C1—P3—C301117.3 (2)C210—C211—H211120.2
C1—P3—C307112.8 (2)C212—C211—H211120.2
C301—P3—C307104.2 (2)C207—C212—C211118.0 (7)
C1—P3—C3109.7 (2)C207—C212—H212121.0
C301—P3—C3106.4 (2)C211—C212—H212121.0
C307—P3—C3105.4 (2)C306—C301—C302118.5 (5)
C407—P4—C401101.6 (2)C306—C301—P3121.0 (4)
C407—P4—C3106.2 (2)C302—C301—P3120.3 (4)
C401—P4—C3102.5 (2)C303—C302—C301120.3 (6)
C407—P4—Ir1117.78 (17)C303—C302—H302119.8
C401—P4—Ir1118.39 (17)C301—C302—H302119.8
C3—P4—Ir1108.78 (16)C304—C303—C302120.2 (7)
C5—O2—C7116.2 (5)C304—C303—H303119.9
C4—C1—P3120.2 (3)C302—C303—H303119.9
C4—C1—P2112.1 (3)C305—C304—C303120.4 (6)
P3—C1—P2124.2 (3)C305—C304—H304119.8
C4—C1—Ir162.6 (2)C303—C304—H304119.8
P3—C1—Ir1110.2 (2)C304—C305—C306119.4 (7)
P2—C1—Ir1109.8 (2)C304—C305—H305120.3
P2—C2—P1111.5 (3)C306—C305—H305120.3
P2—C2—H2A109.3C301—C306—C305121.1 (6)
P1—C2—H2A109.3C301—C306—H306119.4
P2—C2—H2B109.3C305—C306—H306119.4
P1—C2—H2B109.3C312—C307—C308119.3 (5)
H2A—C2—H2B108.0C312—C307—P3121.0 (4)
P3—C3—P4112.7 (3)C308—C307—P3119.4 (4)
P3—C3—H3A109.1C309—C308—C307119.7 (5)
P4—C3—H3A109.1C309—C308—H308120.1
P3—C3—H3B109.1C307—C308—H308120.1
P4—C3—H3B109.1C310—C309—C308120.6 (6)
H3A—C3—H3B107.8C310—C309—H309119.7
C5—C4—C1121.8 (4)C308—C309—H309119.7
C5—C4—Ir1126.1 (3)C311—C310—C309119.8 (6)
C1—C4—Ir176.9 (3)C311—C310—H310120.1
C5—C4—H4111 (3)C309—C310—H310120.1
C1—C4—H4105 (3)C310—C311—C312120.2 (6)
Ir1—C4—H4111 (3)C310—C311—H311119.9
O1—C5—O2123.2 (5)C312—C311—H311119.9
O1—C5—C4126.5 (5)C311—C312—C307120.4 (5)
O2—C5—C4110.2 (5)C311—C312—H312119.8
O2—C7—C8106.0 (6)C307—C312—H312119.8
O2—C7—H7A110.5C402—C401—C406119.9 (5)
C8—C7—H7A110.5C402—C401—P4120.3 (4)
O2—C7—H7B110.5C406—C401—P4119.7 (4)
C8—C7—H7B110.5C401—C402—C403119.7 (5)
H7A—C7—H7B108.7C401—C402—H402120.2
C7—C8—H8A109.5C403—C402—H402120.2
C7—C8—H8B109.5C404—C403—C402120.7 (6)
H8A—C8—H8B109.5C404—C403—H403119.7
C7—C8—H8C109.5C402—C403—H403119.7
H8A—C8—H8C109.5C403—C404—C405119.9 (5)
H8B—C8—H8C109.5C403—C404—H404120.1
C102—C101—C106118.7 (6)C405—C404—H404120.1
C102—C101—P1124.5 (5)C404—C405—C406120.4 (6)
C106—C101—P1116.7 (5)C404—C405—H405119.8
C101—C102—C103121.3 (8)C406—C405—H405119.8
C101—C102—H102119.4C401—C406—C405119.5 (6)
C103—C102—H102119.4C401—C406—H406120.3
C104—C103—C102119.3 (9)C405—C406—H406120.3
C104—C103—H103120.4C412—C407—C408118.9 (5)
C102—C103—H103120.4C412—C407—P4125.1 (5)
C103—C104—C105120.9 (7)C408—C407—P4116.0 (4)
C103—C104—H104119.6C409—C408—C407121.2 (6)
C105—C104—H104119.6C409—C408—H408119.4
C104—C105—C106119.8 (7)C407—C408—H408119.4
C104—C105—H105120.1C410—C409—C408119.8 (7)
C106—C105—H105120.1C410—C409—H409120.1
C101—C106—C105120.0 (7)C408—C409—H409120.1
C101—C106—H106120.0C411—C410—C409119.5 (7)
C105—C106—H106120.0C411—C410—H410120.2
C112—C107—C108119.6 (6)C409—C410—H410120.2
C112—C107—P1118.9 (5)C410—C411—C412121.7 (7)
C108—C107—P1121.5 (5)C410—C411—H411119.2
C107—C108—C109118.0 (8)C412—C411—H411119.2
C107—C108—H108121.0C407—C412—C411118.9 (7)
C109—C108—H108121.0C407—C412—H412120.5
C110—C109—C108120.4 (9)C411—C412—H412120.5
C110—C109—H109119.8Cl3—C9—Cl4118.8 (10)
C108—C109—H109119.8Cl6—C10—Cl5112.1 (5)
C111—C110—C109121.6 (8)Cl7—C11—Cl8110.0 (7)
C111—C110—H110119.2Cl8A—C11—Cl7A94.2 (13)
C109—C110—H110119.2C11—Cl8—Cl9105.0 (7)
C110—C111—C112118.7 (9)Cl10—C12—C12i169 (4)
C110—C111—H111120.6Cl10—C12—Cl9111 (4)
C112—C111—H111120.6C12i—C12—Cl972 (4)
C111—C112—C107121.8 (7)Cl10—C12—Cl9i117 (4)
C111—C112—H112119.1C12i—C12—Cl9i59 (4)
C107—C112—H112119.1Cl9—C12—Cl9i131 (3)
C206—C201—C202119.3 (5)C12—Cl9—Cl8130.1 (14)
C206—C201—P2120.4 (4)C12—Cl9—C12i49 (3)
C202—C201—P2120.2 (4)Cl8—Cl9—C12i138.4 (11)
C203—C202—C201120.2 (6)
C301—P3—C1—C482.4 (4)C201—C202—C203—C2040.8 (9)
C307—P3—C1—C4156.4 (3)C202—C203—C204—C2051.2 (10)
C3—P3—C1—C439.2 (4)C203—C204—C205—C2061.5 (10)
C301—P3—C1—P274.9 (4)C204—C205—C206—C2011.4 (9)
C307—P3—C1—P246.3 (4)C202—C201—C206—C2051.0 (8)
C3—P3—C1—P2163.5 (3)P2—C201—C206—C205178.5 (4)
C301—P3—C1—Ir1151.7 (2)C1—P2—C207—C208164.2 (4)
C307—P3—C1—Ir187.1 (3)C201—P2—C207—C20868.2 (5)
C3—P3—C1—Ir130.1 (3)C2—P2—C207—C20844.0 (5)
C207—P2—C1—C451.6 (4)C1—P2—C207—C21216.3 (5)
C201—P2—C1—C4174.1 (3)C201—P2—C207—C212111.3 (5)
C2—P2—C1—C466.6 (4)C2—P2—C207—C212136.5 (5)
C207—P2—C1—P3107.3 (3)C212—C207—C208—C2091.2 (9)
C201—P2—C1—P315.2 (4)P2—C207—C208—C209179.3 (5)
C2—P2—C1—P3134.5 (3)C207—C208—C209—C2100.2 (12)
C207—P2—C1—Ir1119.1 (2)C208—C209—C210—C2111.5 (13)
C201—P2—C1—Ir1118.4 (2)C209—C210—C211—C2121.4 (12)
C2—P2—C1—Ir10.9 (3)C208—C207—C212—C2111.2 (9)
C1—P2—C2—P128.3 (4)P2—C207—C212—C211179.3 (5)
C207—P2—C2—P193.0 (3)C210—C211—C212—C2070.1 (10)
C201—P2—C2—P1153.9 (3)C1—P3—C301—C30639.5 (5)
C107—P1—C2—P282.4 (3)C307—P3—C301—C30686.1 (5)
C101—P1—C2—P2169.7 (3)C3—P3—C301—C306162.8 (4)
Ir1—P1—C2—P242.7 (3)C1—P3—C301—C302146.1 (4)
C1—P3—C3—P428.1 (4)C307—P3—C301—C30288.3 (5)
C301—P3—C3—P4156.0 (3)C3—P3—C301—C30222.9 (5)
C307—P3—C3—P493.7 (3)C306—C301—C302—C3030.4 (9)
C407—P4—C3—P3114.6 (3)P3—C301—C302—C303174.9 (5)
C401—P4—C3—P3139.3 (3)C301—C302—C303—C3040.6 (11)
Ir1—P4—C3—P313.1 (3)C302—C303—C304—C3051.1 (12)
P3—C1—C4—C526.1 (6)C303—C304—C305—C3060.5 (11)
P2—C1—C4—C5133.8 (4)C302—C301—C306—C3051.0 (9)
Ir1—C1—C4—C5124.6 (5)P3—C301—C306—C305175.4 (5)
P3—C1—C4—Ir198.6 (3)C304—C305—C306—C3010.6 (10)
P2—C1—C4—Ir1101.6 (3)C1—P3—C307—C312121.4 (4)
C7—O2—C5—O13.8 (8)C301—P3—C307—C3127.0 (5)
C7—O2—C5—C4177.9 (5)C3—P3—C307—C312118.9 (4)
C1—C4—C5—O12.7 (8)C1—P3—C307—C30865.1 (5)
Ir1—C4—C5—O194.4 (6)C301—P3—C307—C308166.5 (4)
C1—C4—C5—O2175.6 (4)C3—P3—C307—C30854.6 (5)
Ir1—C4—C5—O287.3 (5)C312—C307—C308—C3090.2 (8)
C5—O2—C7—C8179.9 (6)P3—C307—C308—C309173.4 (5)
C107—P1—C101—C102100.6 (7)C307—C308—C309—C3100.1 (10)
C2—P1—C101—C10210.6 (8)C308—C309—C310—C3110.3 (11)
Ir1—P1—C101—C102125.5 (7)C309—C310—C311—C3120.2 (11)
C107—P1—C101—C10677.3 (6)C310—C311—C312—C3070.1 (10)
C2—P1—C101—C106171.5 (5)C308—C307—C312—C3110.3 (8)
Ir1—P1—C101—C10656.6 (6)P3—C307—C312—C311173.2 (5)
C106—C101—C102—C1030.9 (15)C407—P4—C401—C402121.2 (5)
P1—C101—C102—C103178.7 (9)C3—P4—C401—C402129.1 (4)
C101—C102—C103—C1041.9 (19)Ir1—P4—C401—C4029.5 (5)
C102—C103—C104—C1050.5 (18)C407—P4—C401—C40655.9 (5)
C103—C104—C105—C1061.8 (15)C3—P4—C401—C40653.8 (5)
C102—C101—C106—C1051.4 (12)Ir1—P4—C401—C406173.5 (4)
P1—C101—C106—C105176.6 (6)C406—C401—C402—C4031.5 (9)
C104—C105—C106—C1012.8 (13)P4—C401—C402—C403178.6 (4)
C101—P1—C107—C112102.8 (5)C401—C402—C403—C4040.0 (9)
C2—P1—C107—C112146.0 (4)C402—C403—C404—C4051.0 (10)
Ir1—P1—C107—C11232.0 (5)C403—C404—C405—C4060.5 (11)
C101—P1—C107—C10875.7 (5)C402—C401—C406—C4052.0 (10)
C2—P1—C107—C10835.5 (6)P4—C401—C406—C405179.1 (6)
Ir1—P1—C107—C108149.5 (4)C404—C405—C406—C4011.0 (11)
C112—C107—C108—C1091.0 (10)C401—P4—C407—C41294.0 (6)
P1—C107—C108—C109179.5 (5)C3—P4—C407—C41212.8 (6)
C107—C108—C109—C1101.0 (12)Ir1—P4—C407—C412135.0 (5)
C108—C109—C110—C1110.2 (15)C401—P4—C407—C40883.0 (4)
C109—C110—C111—C1120.6 (14)C3—P4—C407—C408170.2 (4)
C110—C111—C112—C1070.6 (11)Ir1—P4—C407—C40848.0 (4)
C108—C107—C112—C1110.2 (9)C412—C407—C408—C4092.2 (9)
P1—C107—C112—C111178.7 (5)P4—C407—C408—C409175.0 (5)
C1—P2—C201—C206105.6 (4)C407—C408—C409—C4101.9 (9)
C207—P2—C201—C20619.5 (5)C408—C409—C410—C4110.7 (11)
C2—P2—C201—C206132.5 (4)C409—C410—C411—C4123.0 (13)
C1—P2—C201—C20277.0 (5)C408—C407—C412—C4110.1 (10)
C207—P2—C201—C202157.9 (4)P4—C407—C412—C411177.1 (6)
C2—P2—C201—C20244.9 (5)C410—C411—C412—C4072.7 (13)
C206—C201—C202—C2030.8 (8)Cl7—C11—Cl8—Cl9171.2 (8)
P2—C201—C202—C203178.2 (5)
Symmetry code: (i) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2B···Cl20.982.583.488 (5)154
C3—H3A···O10.982.312.892 (7)117
C3—H3B···Cl2ii0.982.833.456 (5)122
Symmetry code: (ii) x1, y, z.
(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}(ethoxyoxoethanylidene)methane-κ4P,C,C',P')chlorido(ethoxyoxoethanido)iridium(III) chloride–methanol–water (1/1/0.5) (5) top
Crystal data top
[Ir(C4H7O2)Cl(C55H50O2P4)]Cl·CH4O·0.5H2OZ = 2
Mr = 1258.07F(000) = 1274
Triclinic, P1Dx = 1.449 Mg m3
a = 12.4253 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.7081 (4) ÅCell parameters from 57775 reflections
c = 17.6780 (6) Åθ = 1.0–22.5°
α = 93.152 (2)°µ = 2.57 mm1
β = 97.960 (2)°T = 233 K
γ = 103.771 (2)°Plate, colorless
V = 2884.18 (15) Å30.15 × 0.05 × 0.02 mm
Data collection top
Nonius KappaCCD
diffractometer
6326 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.037
Graphite monochromatorθmax = 22.4°, θmin = 1.9°
phi– and ω–scansh = 1313
13821 measured reflectionsk = 1414
7453 independent reflectionsl = 1818
Refinement top
Refinement on F21 restraint
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.044H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.106 w = 1/[σ2(Fo2) + (0.047P)2 + 6.9463P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
7453 reflectionsΔρmax = 0.90 e Å3
674 parametersΔρmin = 0.96 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Small crystal with low diffraction, but good quality. Reflections were collected only until 45 degrees (2Theta). Hydrogen at C4 was found and refined isotropically with bond restraint (d=0.96 angs.). Solvent molecules methanole and water lies nearby an inversion centre and were all refined with multipicity of 0.5 (C12-O5, C13-O6 and O7). Hydrogens of these disordered molecules were not exact logalized and omitted. A 1:1 positional disorder occurs for one phenyl group of the phospane (C401-C406 and C41A-C46A). The distance of the carbon atoms between disordered rings are small and all atoms were refined isotropically.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ir10.16510 (2)0.10634 (2)0.69970 (2)0.04147 (12)
P10.15686 (15)0.26886 (16)0.72460 (11)0.0454 (5)
P20.35224 (14)0.24371 (15)0.79978 (10)0.0416 (5)
P30.35696 (14)0.02021 (14)0.78288 (10)0.0414 (5)
P40.17014 (15)0.05959 (16)0.68972 (11)0.0474 (5)
Cl10.00070 (14)0.05642 (16)0.80140 (11)0.0558 (5)
Cl20.3358 (4)0.3182 (3)0.8216 (2)0.1433 (14)
C10.3307 (5)0.1353 (5)0.7465 (4)0.0389 (16)
C20.2231 (6)0.2821 (6)0.8122 (4)0.0479 (19)
H2A0.23780.35260.82420.057*
H2B0.17160.24070.85550.057*
C30.2880 (6)0.0839 (5)0.7350 (4)0.053 (2)
H3A0.25970.14320.77220.063*
H3B0.34330.09960.69540.063*
C1010.0247 (6)0.3050 (6)0.7536 (4)0.053 (2)
C1020.0243 (7)0.3454 (7)0.6989 (5)0.073 (3)
H1020.00940.35220.64730.088*
C1030.1207 (8)0.3760 (8)0.7172 (6)0.088 (3)
H1030.15160.40450.67850.106*
C1040.1718 (7)0.3654 (8)0.7907 (7)0.088 (3)
H1040.23760.38730.80340.106*
C1050.1274 (8)0.3226 (9)0.8466 (6)0.091 (3)
H1050.16380.31370.89770.110*
C1060.0293 (7)0.2922 (7)0.8284 (5)0.073 (3)
H1060.00070.26280.86710.087*
C1070.2385 (6)0.3784 (6)0.6601 (4)0.0460 (19)
C1080.2860 (5)0.3683 (6)0.5870 (4)0.0445 (18)
H1080.27450.30430.56840.053*
C1090.3505 (7)0.4520 (7)0.5407 (5)0.061 (2)
H1090.38400.44440.49110.073*
C1100.3662 (7)0.5465 (7)0.5666 (5)0.064 (2)
H1100.40970.60310.53450.077*
C1110.3188 (8)0.5580 (7)0.6388 (6)0.069 (2)
H1110.33050.62240.65680.083*
C1120.2531 (7)0.4745 (7)0.6857 (5)0.060 (2)
H1120.21850.48270.73490.072*
C2010.3904 (6)0.2312 (5)0.8937 (4)0.0448 (18)
C2020.5033 (6)0.2505 (6)0.9013 (4)0.053 (2)
H2020.55790.26580.85700.064*
C2030.5363 (8)0.2477 (6)0.9718 (5)0.066 (2)
H2030.61290.26020.97580.079*
C2040.4576 (8)0.2267 (7)1.0364 (5)0.072 (3)
H2040.48040.22671.08490.086*
C2050.3439 (9)0.2053 (7)1.0310 (5)0.074 (3)
H2050.29000.18841.07560.089*
C2060.3110 (7)0.2089 (6)0.9600 (4)0.060 (2)
H2060.23420.19630.95620.073*
C2070.4620 (6)0.3491 (6)0.7494 (4)0.0446 (18)
C2080.5408 (5)0.3389 (6)0.6880 (4)0.0462 (18)
H2080.53740.27560.66920.055*
C2090.6234 (6)0.4213 (7)0.6548 (5)0.056 (2)
H2090.67670.41450.61350.068*
C2100.6281 (7)0.5149 (7)0.6825 (5)0.070 (3)
H2100.68440.57130.65930.083*
C2110.5522 (8)0.5262 (7)0.7431 (6)0.072 (3)
H2110.55630.58970.76180.086*
C2120.4681 (7)0.4419 (6)0.7769 (5)0.058 (2)
H2120.41540.44870.81860.069*
C3010.5010 (6)0.0138 (6)0.7748 (4)0.0418 (17)
C3020.5909 (6)0.0976 (6)0.7612 (4)0.053 (2)
H3020.57750.16200.75480.064*
C3030.6999 (6)0.0886 (7)0.7567 (5)0.062 (2)
H3030.76000.14650.74810.074*
C3040.7200 (6)0.0057 (8)0.7648 (4)0.060 (2)
H3040.79410.01230.76140.072*
C3050.6329 (7)0.0893 (7)0.7777 (4)0.057 (2)
H3050.64720.15340.78240.068*
C3060.5232 (6)0.0807 (6)0.7838 (4)0.052 (2)
H3060.46360.13890.79410.063*
C3070.3001 (6)0.0081 (6)0.8841 (4)0.0466 (19)
C3080.1853 (6)0.0207 (7)0.9072 (5)0.071 (3)
H3080.13900.01060.87120.085*
C3090.1405 (7)0.0481 (8)0.9833 (5)0.084 (3)
H3090.06300.05740.99870.101*
C3100.2066 (7)0.0621 (7)1.0376 (5)0.071 (3)
H3100.17530.07951.08950.085*
C3110.3204 (6)0.0499 (6)1.0135 (4)0.059 (2)
H3110.36640.05981.04970.071*
C3120.3670 (6)0.0239 (6)0.9383 (4)0.0493 (19)
H3120.44430.01670.92310.059*
C4070.1952 (5)0.1127 (6)0.5980 (4)0.0473 (19)
C4080.2121 (6)0.0529 (6)0.5294 (4)0.056 (2)
H4080.21110.01550.52950.067*
C4090.2304 (8)0.0951 (8)0.4601 (5)0.071 (2)
H4090.24100.05470.41370.085*
C4100.2332 (8)0.1947 (8)0.4586 (6)0.074 (3)
H4100.24640.22230.41170.088*
C4110.2163 (7)0.2534 (7)0.5275 (7)0.076 (3)
H4110.21760.32160.52690.091*
C4120.1977 (7)0.2145 (7)0.5966 (5)0.064 (2)
H4120.18660.25570.64270.076*
O10.4427 (5)0.0485 (4)0.6132 (3)0.0596 (14)
O20.4118 (4)0.1706 (4)0.5351 (3)0.0514 (13)
O30.1320 (7)0.1339 (6)0.4883 (4)0.100 (2)
O40.0633 (4)0.2499 (4)0.5440 (3)0.0587 (14)
C40.3334 (6)0.1604 (5)0.6621 (4)0.0390 (17)
H40.353 (4)0.2318 (16)0.654 (3)0.011 (13)*
C50.4024 (5)0.1187 (6)0.6027 (4)0.0411 (17)
C60.4691 (7)0.1344 (7)0.4686 (4)0.063 (2)
H6A0.44170.06120.46850.075*
H6B0.55020.15090.46860.075*
C70.4415 (9)0.1883 (8)0.4004 (5)0.088 (3)
H7A0.47710.16770.35370.131*
H7B0.36090.17140.40170.131*
H7C0.46870.26050.40180.131*
C80.0453 (6)0.1001 (6)0.6211 (4)0.054 (2)
H8A0.01630.02920.61260.064*
H8B0.01790.12370.64640.064*
C90.0851 (7)0.1581 (7)0.5455 (5)0.059 (2)
C100.0925 (8)0.3085 (7)0.4698 (5)0.074 (3)
H10A0.04830.27370.43300.088*
H10B0.17220.31690.45010.088*
C110.0689 (8)0.4077 (7)0.4797 (6)0.093 (3)
H11A0.08790.44810.43070.140*
H11B0.01020.39860.49890.140*
H11C0.11340.44160.51590.140*
O50.2422 (14)0.5220 (9)0.8989 (9)0.107 (5)0.5
C120.190 (5)0.564 (4)0.9732 (15)0.25 (3)0.5
O60.5573 (15)0.4914 (9)1.0173 (8)0.101 (5)0.5
C130.665 (6)0.4857 (18)0.979 (2)0.28 (4)0.5
O70.3475 (17)0.5078 (11)1.0734 (10)0.113 (6)0.5
C4010.0507 (14)0.1668 (14)0.7345 (10)0.039 (5)*0.5
C4020.0572 (18)0.2344 (16)0.7933 (12)0.083 (6)*0.5
H4020.12410.23270.81300.099*0.5
C4030.044 (2)0.3058 (19)0.8217 (15)0.108 (7)*0.5
H4030.04420.35170.86330.129*0.5
C4040.137 (2)0.3123 (17)0.7935 (12)0.085 (6)*0.5
H4040.19970.36630.81200.102*0.5
C4050.1458 (16)0.2471 (15)0.7416 (14)0.055 (5)*0.5
H4050.21330.25010.72230.065*0.5
C4060.047 (2)0.1700 (17)0.7148 (14)0.065 (8)*0.5
H4060.05280.11730.68030.077*0.5
C41A0.0372 (18)0.1384 (16)0.7366 (12)0.055 (7)*0.5
C42A0.0192 (18)0.1861 (15)0.8085 (12)0.079 (6)*0.5
H42A0.07850.17770.83730.095*0.5
C43A0.093 (2)0.2514 (18)0.8423 (15)0.103 (7)*0.5
H43A0.10970.27860.89380.123*0.5
C44A0.171 (2)0.2690 (18)0.7943 (14)0.083 (6)*0.5
H44A0.24100.31230.81370.100*0.5
C45A0.1536 (17)0.2269 (15)0.7166 (12)0.062 (6)*0.5
H45A0.20950.24220.68530.074*0.5
C46A0.0517 (15)0.1634 (13)0.6908 (12)0.037 (5)*0.5
H46A0.03800.13390.64000.045*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.02378 (16)0.0610 (2)0.03666 (18)0.00846 (12)0.00368 (11)0.00960 (13)
P10.0282 (10)0.0686 (14)0.0392 (11)0.0161 (9)0.0022 (8)0.0081 (9)
P20.0285 (9)0.0612 (13)0.0326 (10)0.0099 (9)0.0029 (8)0.0066 (9)
P30.0307 (10)0.0554 (12)0.0360 (10)0.0092 (9)0.0059 (8)0.0092 (9)
P40.0311 (10)0.0633 (13)0.0418 (11)0.0025 (9)0.0069 (9)0.0082 (9)
Cl10.0271 (9)0.0823 (14)0.0511 (12)0.0104 (9)0.0032 (8)0.0146 (10)
Cl20.170 (4)0.105 (3)0.150 (3)0.013 (2)0.049 (3)0.001 (2)
C10.028 (4)0.055 (4)0.034 (4)0.014 (3)0.001 (3)0.004 (3)
C20.039 (4)0.070 (5)0.034 (4)0.018 (4)0.000 (3)0.009 (4)
C30.055 (5)0.049 (5)0.055 (5)0.008 (4)0.025 (4)0.005 (4)
C1010.034 (4)0.075 (6)0.052 (5)0.022 (4)0.001 (4)0.007 (4)
C1020.048 (5)0.117 (8)0.059 (6)0.038 (5)0.002 (4)0.010 (5)
C1030.058 (6)0.124 (9)0.088 (8)0.048 (6)0.001 (6)0.025 (6)
C1040.046 (5)0.113 (9)0.115 (9)0.044 (6)0.001 (6)0.003 (7)
C1050.058 (6)0.137 (10)0.078 (7)0.041 (6)0.018 (5)0.004 (7)
C1060.052 (5)0.110 (8)0.059 (6)0.036 (5)0.003 (5)0.007 (5)
C1070.037 (4)0.055 (5)0.047 (5)0.016 (4)0.006 (4)0.009 (4)
C1080.034 (4)0.056 (5)0.040 (5)0.010 (4)0.003 (3)0.015 (4)
C1090.050 (5)0.076 (7)0.056 (5)0.025 (5)0.006 (4)0.019 (5)
C1100.051 (5)0.068 (7)0.068 (6)0.009 (4)0.009 (5)0.023 (5)
C1110.072 (6)0.055 (6)0.078 (7)0.015 (5)0.010 (5)0.009 (5)
C1120.063 (5)0.071 (6)0.053 (5)0.029 (5)0.012 (4)0.000 (5)
C2010.045 (4)0.058 (5)0.030 (4)0.012 (4)0.004 (3)0.003 (3)
C2020.044 (5)0.075 (6)0.042 (5)0.016 (4)0.008 (4)0.000 (4)
C2030.064 (6)0.081 (6)0.058 (6)0.018 (5)0.027 (5)0.006 (5)
C2040.085 (7)0.077 (6)0.057 (6)0.017 (5)0.034 (6)0.006 (5)
C2050.091 (7)0.098 (7)0.038 (5)0.036 (6)0.006 (5)0.003 (5)
C2060.059 (5)0.080 (6)0.044 (5)0.023 (5)0.008 (4)0.004 (4)
C2070.035 (4)0.052 (5)0.044 (4)0.007 (3)0.009 (4)0.011 (4)
C2080.031 (4)0.058 (5)0.045 (4)0.006 (4)0.003 (4)0.013 (4)
C2090.038 (4)0.072 (6)0.053 (5)0.003 (4)0.013 (4)0.012 (4)
C2100.056 (6)0.077 (7)0.060 (6)0.011 (5)0.012 (5)0.018 (5)
C2110.071 (6)0.063 (6)0.079 (7)0.007 (5)0.020 (6)0.004 (5)
C2120.056 (5)0.056 (6)0.057 (5)0.005 (4)0.008 (4)0.008 (4)
C3010.035 (4)0.058 (5)0.034 (4)0.016 (4)0.006 (3)0.002 (3)
C3020.039 (4)0.065 (5)0.056 (5)0.013 (4)0.011 (4)0.008 (4)
C3030.028 (4)0.089 (7)0.058 (5)0.001 (4)0.001 (4)0.006 (5)
C3040.032 (4)0.106 (7)0.048 (5)0.027 (5)0.008 (4)0.000 (5)
C3050.050 (5)0.080 (6)0.050 (5)0.034 (5)0.010 (4)0.001 (4)
C3060.047 (5)0.071 (6)0.039 (4)0.017 (4)0.005 (4)0.005 (4)
C3070.036 (4)0.064 (5)0.037 (4)0.010 (4)0.007 (3)0.011 (4)
C3080.036 (5)0.110 (7)0.060 (6)0.020 (5)0.003 (4)0.031 (5)
C3090.041 (5)0.136 (9)0.062 (6)0.025 (5)0.017 (5)0.045 (6)
C3100.056 (5)0.108 (7)0.045 (5)0.027 (5)0.005 (4)0.028 (5)
C3110.045 (5)0.089 (6)0.042 (5)0.019 (4)0.006 (4)0.012 (4)
C3120.034 (4)0.073 (5)0.038 (4)0.014 (4)0.003 (3)0.011 (4)
C4070.023 (4)0.061 (5)0.057 (5)0.006 (3)0.010 (3)0.002 (4)
C4080.051 (5)0.070 (6)0.046 (5)0.012 (4)0.011 (4)0.000 (4)
C4090.074 (6)0.085 (7)0.055 (6)0.019 (5)0.019 (5)0.002 (5)
C4100.070 (6)0.092 (8)0.066 (6)0.026 (6)0.019 (5)0.022 (6)
C4110.060 (6)0.069 (6)0.106 (9)0.022 (5)0.018 (6)0.022 (6)
C4120.053 (5)0.070 (6)0.066 (6)0.019 (4)0.002 (4)0.008 (5)
O10.066 (4)0.072 (4)0.054 (3)0.038 (3)0.015 (3)0.004 (3)
O20.055 (3)0.064 (3)0.035 (3)0.022 (3)0.004 (2)0.006 (2)
O30.144 (7)0.126 (6)0.052 (4)0.081 (6)0.010 (4)0.003 (4)
O40.052 (3)0.072 (4)0.051 (3)0.016 (3)0.009 (3)0.008 (3)
C40.038 (4)0.045 (5)0.034 (4)0.010 (3)0.012 (3)0.008 (3)
C50.029 (4)0.058 (5)0.038 (4)0.011 (4)0.007 (3)0.002 (4)
C60.050 (5)0.097 (7)0.042 (5)0.023 (5)0.002 (4)0.016 (4)
C70.101 (8)0.117 (8)0.039 (5)0.022 (7)0.001 (5)0.008 (5)
C80.039 (4)0.066 (5)0.054 (5)0.012 (4)0.008 (4)0.017 (4)
C90.044 (5)0.076 (6)0.059 (6)0.019 (4)0.014 (4)0.007 (5)
C100.073 (6)0.088 (7)0.057 (6)0.019 (5)0.016 (5)0.024 (5)
C110.080 (7)0.079 (7)0.116 (9)0.011 (6)0.029 (6)0.037 (6)
O50.156 (15)0.052 (8)0.109 (12)0.022 (9)0.004 (10)0.027 (8)
C120.49 (8)0.31 (5)0.030 (15)0.29 (6)0.03 (3)0.00 (2)
O60.182 (18)0.053 (8)0.064 (10)0.025 (10)0.004 (10)0.029 (7)
C130.59 (10)0.038 (13)0.09 (2)0.02 (3)0.21 (4)0.016 (15)
O70.164 (16)0.067 (10)0.078 (11)0.018 (10)0.002 (11)0.006 (9)
Geometric parameters (Å, º) top
Ir1—C42.046 (7)C304—H3040.9400
Ir1—C82.163 (7)C305—C3061.385 (10)
Ir1—C12.279 (6)C305—H3050.9400
Ir1—P42.306 (2)C306—H3060.9400
Ir1—P12.318 (2)C307—C3121.392 (9)
Ir1—Cl12.4607 (18)C307—C3081.395 (10)
P1—C1071.831 (7)C308—C3091.378 (11)
P1—C1011.840 (7)C308—H3080.9400
P1—C21.850 (7)C309—C3101.380 (11)
P2—C11.788 (7)C309—H3090.9400
P2—C21.794 (7)C310—C3111.385 (11)
P2—C2011.799 (7)C310—H3100.9400
P2—C2071.823 (7)C311—C3121.366 (10)
P3—C11.789 (7)C311—H3110.9400
P3—C3011.799 (7)C312—H3120.9400
P3—C31.800 (7)C407—C4081.388 (10)
P3—C3071.816 (7)C407—C4121.404 (11)
P4—C41A1.80 (2)C408—C4091.396 (11)
P4—C4071.832 (8)C408—H4080.9400
P4—C31.850 (7)C409—C4101.375 (12)
P4—C4011.871 (18)C409—H4090.9400
C1—C41.507 (9)C410—C4111.385 (13)
C2—H2A0.9800C410—H4100.9400
C2—H2B0.9800C411—C4121.372 (12)
C3—H3A0.9800C411—H4110.9400
C3—H3B0.9800C412—H4120.9400
C101—C1021.371 (10)O1—C51.203 (8)
C101—C1061.378 (11)O2—C51.332 (8)
C102—C1031.364 (11)O2—C61.461 (8)
C102—H1020.9400O3—C91.199 (10)
C103—C1041.350 (13)O4—C91.348 (10)
C103—H1030.9400O4—C101.453 (9)
C104—C1051.366 (13)C4—C51.488 (10)
C104—H1040.9400C4—H40.947 (19)
C105—C1061.382 (12)C6—C71.500 (11)
C105—H1050.9400C6—H6A0.9800
C106—H1060.9400C6—H6B0.9800
C107—C1081.373 (10)C7—H7A0.9700
C107—C1121.395 (11)C7—H7B0.9700
C108—C1091.380 (10)C7—H7C0.9700
C108—H1080.9400C8—C91.475 (11)
C109—C1101.377 (12)C8—H8A0.9800
C109—H1090.9400C8—H8B0.9800
C110—C1111.363 (12)C10—C111.472 (13)
C110—H1100.9400C10—H10A0.9800
C111—C1121.388 (12)C10—H10B0.9800
C111—H1110.9400C11—H11A0.9700
C112—H1120.9400C11—H11B0.9700
C201—C2021.391 (10)C11—H11C0.9700
C201—C2061.393 (10)O5—C121.41 (3)
C202—C2031.366 (10)O6—C131.39 (6)
C202—H2020.9400O6—O6i1.60 (3)
C203—C2041.366 (12)C13—O7i0.96 (5)
C203—H2030.9400O7—C13i0.96 (5)
C204—C2051.390 (12)C401—C4061.30 (3)
C204—H2040.9400C401—C4021.38 (3)
C205—C2061.375 (11)C402—C4031.40 (3)
C205—H2050.9400C402—H4020.9400
C206—H2060.9400C403—C4041.32 (3)
C207—C2121.376 (10)C403—H4030.9400
C207—C2081.394 (10)C404—C4051.28 (3)
C208—C2091.371 (10)C404—H4040.9400
C208—H2080.9400C405—C4061.42 (3)
C209—C2101.389 (12)C405—H4050.9400
C209—H2090.9400C406—H4060.9400
C210—C2111.368 (12)C41A—C42A1.36 (3)
C210—H2100.9400C41A—C46A1.45 (3)
C211—C2121.400 (12)C42A—C43A1.49 (3)
C211—H2110.9400C42A—H42A0.9400
C212—H2120.9400C43A—C44A1.36 (3)
C301—C3021.382 (10)C43A—H43A0.9400
C301—C3061.393 (10)C44A—C45A1.43 (3)
C302—C3031.381 (10)C44A—H44A0.9400
C302—H3020.9400C45A—C46A1.36 (3)
C303—C3041.378 (11)C45A—H45A0.9400
C303—H3030.9400C46A—H46A0.9400
C304—C3051.359 (11)
C4—Ir1—C8120.8 (3)C306—C301—P3118.3 (6)
C4—Ir1—C140.3 (2)C303—C302—C301121.4 (8)
C8—Ir1—C1161.1 (3)C303—C302—H302119.3
C4—Ir1—P493.6 (2)C301—C302—H302119.3
C8—Ir1—P493.0 (2)C304—C303—C302119.6 (8)
C1—Ir1—P489.61 (18)C304—C303—H303120.2
C4—Ir1—P188.5 (2)C302—C303—H303120.2
C8—Ir1—P191.2 (2)C305—C304—C303120.1 (7)
C1—Ir1—P188.02 (18)C305—C304—H304120.0
P4—Ir1—P1173.53 (7)C303—C304—H304120.0
C4—Ir1—Cl1152.49 (19)C304—C305—C306120.7 (8)
C8—Ir1—Cl185.9 (2)C304—C305—H305119.7
C1—Ir1—Cl1112.78 (17)C306—C305—H305119.7
P4—Ir1—Cl191.38 (7)C305—C306—C301120.2 (8)
P1—Ir1—Cl184.00 (7)C305—C306—H306119.9
C107—P1—C101101.9 (3)C301—C306—H306119.9
C107—P1—C2103.5 (3)C312—C307—C308119.4 (7)
C101—P1—C2102.5 (3)C312—C307—P3121.5 (5)
C107—P1—Ir1121.5 (3)C308—C307—P3118.9 (5)
C101—P1—Ir1123.4 (3)C309—C308—C307119.2 (7)
C2—P1—Ir1100.7 (3)C309—C308—H308120.4
C1—P2—C2107.0 (3)C307—C308—H308120.4
C1—P2—C201118.4 (3)C308—C309—C310121.7 (8)
C2—P2—C201106.6 (3)C308—C309—H309119.2
C1—P2—C207112.4 (3)C310—C309—H309119.2
C2—P2—C207108.0 (3)C309—C310—C311118.3 (7)
C201—P2—C207104.0 (3)C309—C310—H310120.9
C1—P3—C301117.2 (3)C311—C310—H310120.9
C1—P3—C3110.5 (3)C312—C311—C310121.4 (7)
C301—P3—C3105.7 (4)C312—C311—H311119.3
C1—P3—C307110.7 (3)C310—C311—H311119.3
C301—P3—C307105.7 (3)C311—C312—C307120.0 (7)
C3—P3—C307106.5 (4)C311—C312—H312120.0
C41A—P4—C407104.1 (7)C307—C312—H312120.0
C41A—P4—C3111.6 (7)C408—C407—C412119.5 (7)
C407—P4—C3100.5 (3)C408—C407—P4120.4 (6)
C407—P4—C40196.0 (6)C412—C407—P4120.1 (6)
C3—P4—C401102.3 (6)C407—C408—C409119.4 (8)
C41A—P4—Ir1108.0 (7)C407—C408—H408120.3
C407—P4—Ir1123.5 (3)C409—C408—H408120.3
C3—P4—Ir1108.9 (2)C410—C409—C408121.2 (8)
C401—P4—Ir1122.0 (6)C410—C409—H409119.4
C4—C1—P2113.5 (5)C408—C409—H409119.4
C4—C1—P3121.9 (5)C409—C410—C411118.6 (9)
P2—C1—P3120.6 (4)C409—C410—H410120.7
C4—C1—Ir161.5 (3)C411—C410—H410120.7
P2—C1—Ir1112.4 (3)C412—C411—C410121.7 (9)
P3—C1—Ir1111.3 (3)C412—C411—H411119.2
P2—C2—P1111.0 (4)C410—C411—H411119.2
P2—C2—H2A109.4C411—C412—C407119.5 (8)
P1—C2—H2A109.4C411—C412—H412120.2
P2—C2—H2B109.4C407—C412—H412120.2
P1—C2—H2B109.4C5—O2—C6116.8 (6)
H2A—C2—H2B108.0C9—O4—C10115.6 (7)
P3—C3—P4113.8 (4)C5—C4—C1121.8 (6)
P3—C3—H3A108.8C5—C4—Ir1126.1 (5)
P4—C3—H3A108.8C1—C4—Ir178.2 (4)
P3—C3—H3B108.8C5—C4—H4110 (3)
P4—C3—H3B108.8C1—C4—H4106 (3)
H3A—C3—H3B107.7Ir1—C4—H4111 (3)
C102—C101—C106117.6 (7)O1—C5—O2124.9 (6)
C102—C101—P1119.2 (6)O1—C5—C4125.8 (6)
C106—C101—P1123.2 (6)O2—C5—C4109.4 (6)
C103—C102—C101121.9 (9)O2—C6—C7104.9 (6)
C103—C102—H102119.1O2—C6—H6A110.8
C101—C102—H102119.1C7—C6—H6A110.8
C104—C103—C102120.2 (9)O2—C6—H6B110.8
C104—C103—H103119.9C7—C6—H6B110.8
C102—C103—H103119.9H6A—C6—H6B108.8
C103—C104—C105119.7 (8)C6—C7—H7A109.5
C103—C104—H104120.2C6—C7—H7B109.5
C105—C104—H104120.2H7A—C7—H7B109.5
C104—C105—C106120.3 (9)C6—C7—H7C109.5
C104—C105—H105119.9H7A—C7—H7C109.5
C106—C105—H105119.9H7B—C7—H7C109.5
C101—C106—C105120.3 (8)C9—C8—Ir1117.5 (5)
C101—C106—H106119.8C9—C8—H8A107.9
C105—C106—H106119.8Ir1—C8—H8A107.9
C108—C107—C112119.1 (7)C9—C8—H8B107.9
C108—C107—P1121.5 (6)Ir1—C8—H8B107.9
C112—C107—P1119.4 (6)H8A—C8—H8B107.2
C107—C108—C109120.1 (8)O3—C9—O4118.8 (8)
C107—C108—H108119.9O3—C9—C8128.8 (9)
C109—C108—H108119.9O4—C9—C8112.4 (8)
C110—C109—C108120.6 (8)O4—C10—C11108.2 (8)
C110—C109—H109119.7O4—C10—H10A110.1
C108—C109—H109119.7C11—C10—H10A110.1
C111—C110—C109120.0 (8)O4—C10—H10B110.1
C111—C110—H110120.0C11—C10—H10B110.1
C109—C110—H110120.0H10A—C10—H10B108.4
C110—C111—C112119.9 (9)C10—C11—H11A109.5
C110—C111—H111120.0C10—C11—H11B109.5
C112—C111—H111120.0H11A—C11—H11B109.5
C111—C112—C107120.1 (8)C10—C11—H11C109.5
C111—C112—H112119.9H11A—C11—H11C109.5
C107—C112—H112119.9H11B—C11—H11C109.5
C202—C201—C206118.4 (7)C13—O6—O6i128 (3)
C202—C201—P2119.3 (5)O7i—C13—O6103 (7)
C206—C201—P2122.2 (6)C406—C401—C402118 (2)
C203—C202—C201121.3 (8)C406—C401—P4117.2 (16)
C203—C202—H202119.4C402—C401—P4123.9 (14)
C201—C202—H202119.4C401—C402—C403115 (2)
C204—C203—C202119.8 (8)C401—C402—H402122.5
C204—C203—H203120.1C403—C402—H402122.5
C202—C203—H203120.1C404—C403—C402124 (2)
C203—C204—C205120.5 (8)C404—C403—H403118.1
C203—C204—H204119.7C402—C403—H403118.1
C205—C204—H204119.7C405—C404—C403122 (2)
C206—C205—C204119.5 (9)C405—C404—H404119.2
C206—C205—H205120.2C403—C404—H404119.2
C204—C205—H205120.2C404—C405—C406116 (2)
C205—C206—C201120.5 (8)C404—C405—H405122.1
C205—C206—H206119.8C406—C405—H405122.1
C201—C206—H206119.8C401—C406—C405125 (2)
C212—C207—C208119.7 (7)C401—C406—H406117.7
C212—C207—P2116.7 (6)C405—C406—H406117.7
C208—C207—P2123.5 (6)C42A—C41A—C46A118 (2)
C209—C208—C207120.1 (8)C42A—C41A—P4124.6 (17)
C209—C208—H208120.0C46A—C41A—P4117.3 (15)
C207—C208—H208120.0C41A—C42A—C43A121 (2)
C208—C209—C210119.8 (8)C41A—C42A—H42A119.5
C208—C209—H209120.1C43A—C42A—H42A119.5
C210—C209—H209120.1C44A—C43A—C42A116 (2)
C211—C210—C209121.0 (8)C44A—C43A—H43A122.1
C211—C210—H210119.5C42A—C43A—H43A122.1
C209—C210—H210119.5C43A—C44A—C45A125 (2)
C210—C211—C212119.0 (9)C43A—C44A—H44A117.4
C210—C211—H211120.5C45A—C44A—H44A117.4
C212—C211—H211120.5C46A—C45A—C44A116 (2)
C207—C212—C211120.4 (8)C46A—C45A—H45A122.1
C207—C212—H212119.8C44A—C45A—H45A122.1
C211—C212—H212119.8C45A—C46A—C41A124 (2)
C302—C301—C306118.1 (6)C45A—C46A—H46A118.0
C302—C301—P3123.6 (5)C41A—C46A—H46A118.0
C2—P2—C1—C477.0 (5)C307—P3—C301—C302106.7 (6)
C201—P2—C1—C4162.8 (5)C1—P3—C301—C306163.7 (5)
C207—P2—C1—C441.4 (5)C3—P3—C301—C30640.2 (6)
C2—P2—C1—P3124.9 (4)C307—P3—C301—C30672.5 (6)
C201—P2—C1—P34.7 (5)C306—C301—C302—C3030.2 (11)
C207—P2—C1—P3116.6 (4)P3—C301—C302—C303179.0 (6)
C2—P2—C1—Ir19.6 (4)C301—C302—C303—C3041.0 (12)
C201—P2—C1—Ir1129.8 (3)C302—C303—C304—C3050.5 (12)
C207—P2—C1—Ir1108.9 (3)C303—C304—C305—C3060.9 (12)
C301—P3—C1—C479.1 (6)C304—C305—C306—C3011.7 (11)
C3—P3—C1—C442.0 (6)C302—C301—C306—C3051.2 (10)
C307—P3—C1—C4159.7 (5)P3—C301—C306—C305179.6 (6)
C301—P3—C1—P277.1 (5)C1—P3—C307—C312124.5 (6)
C3—P3—C1—P2161.8 (4)C301—P3—C307—C3123.4 (7)
C307—P3—C1—P244.1 (5)C3—P3—C307—C312115.5 (7)
C301—P3—C1—Ir1147.9 (3)C1—P3—C307—C30859.7 (8)
C3—P3—C1—Ir126.9 (4)C301—P3—C307—C308172.4 (7)
C307—P3—C1—Ir190.8 (4)C3—P3—C307—C30860.4 (8)
C1—P2—C2—P139.1 (5)C312—C307—C308—C3090.3 (14)
C201—P2—C2—P1166.6 (4)P3—C307—C308—C309176.2 (8)
C207—P2—C2—P182.2 (5)C307—C308—C309—C3100.8 (16)
C107—P1—C2—P277.5 (5)C308—C309—C310—C3111.2 (16)
C101—P1—C2—P2176.8 (4)C309—C310—C311—C3120.5 (14)
Ir1—P1—C2—P248.8 (4)C310—C311—C312—C3070.6 (13)
C1—P3—C3—P421.3 (6)C308—C307—C312—C3111.0 (12)
C301—P3—C3—P4149.0 (4)P3—C307—C312—C311176.8 (6)
C307—P3—C3—P498.9 (4)C41A—P4—C407—C408123.0 (9)
C41A—P4—C3—P3112.8 (8)C3—P4—C407—C408121.4 (6)
C407—P4—C3—P3137.3 (4)C401—P4—C407—C408134.9 (8)
C401—P4—C3—P3124.2 (7)Ir1—P4—C407—C4080.3 (7)
Ir1—P4—C3—P36.2 (5)C41A—P4—C407—C41257.1 (9)
C107—P1—C101—C10245.5 (8)C3—P4—C407—C41258.5 (6)
C2—P1—C101—C102152.5 (7)C401—P4—C407—C41245.2 (8)
Ir1—P1—C101—C10295.6 (7)Ir1—P4—C407—C412179.6 (5)
C107—P1—C101—C106135.4 (8)C412—C407—C408—C4090.4 (11)
C2—P1—C101—C10628.4 (9)P4—C407—C408—C409179.6 (6)
Ir1—P1—C101—C10683.6 (8)C407—C408—C409—C4100.6 (12)
C106—C101—C102—C1032.6 (15)C408—C409—C410—C4110.6 (13)
P1—C101—C102—C103178.3 (8)C409—C410—C411—C4120.4 (14)
C101—C102—C103—C1041.2 (17)C410—C411—C412—C4070.2 (13)
C102—C103—C104—C1050.9 (18)C408—C407—C412—C4110.2 (11)
C103—C104—C105—C1061.4 (17)P4—C407—C412—C411179.9 (6)
C102—C101—C106—C1052.0 (15)P2—C1—C4—C5130.9 (6)
P1—C101—C106—C105178.9 (8)P3—C1—C4—C526.8 (9)
C104—C105—C106—C1010.0 (17)Ir1—C1—C4—C5125.4 (7)
C101—P1—C107—C108126.6 (6)P2—C1—C4—Ir1103.7 (4)
C2—P1—C107—C108127.3 (6)P3—C1—C4—Ir198.5 (5)
Ir1—P1—C107—C10815.5 (7)C6—O2—C5—O14.3 (10)
C101—P1—C107—C11253.6 (6)C6—O2—C5—C4175.0 (6)
C2—P1—C107—C11252.5 (6)C1—C4—C5—O115.8 (11)
Ir1—P1—C107—C112164.3 (5)Ir1—C4—C5—O183.0 (8)
C112—C107—C108—C1092.2 (10)C1—C4—C5—O2164.9 (6)
P1—C107—C108—C109177.6 (5)Ir1—C4—C5—O296.2 (6)
C107—C108—C109—C1101.3 (11)C5—O2—C6—C7165.9 (7)
C108—C109—C110—C1110.7 (12)C10—O4—C9—O34.3 (11)
C109—C110—C111—C1121.0 (12)C10—O4—C9—C8175.6 (7)
C110—C111—C112—C1072.0 (12)Ir1—C8—C9—O384.8 (11)
C108—C107—C112—C1112.6 (11)Ir1—C8—C9—O495.3 (7)
P1—C107—C112—C111177.2 (6)C9—O4—C10—C11177.0 (7)
C1—P2—C201—C20290.5 (7)O6i—O6—C13—O7i2 (4)
C2—P2—C201—C202149.0 (6)C407—P4—C401—C40679.1 (17)
C207—P2—C201—C20235.1 (7)C3—P4—C401—C406178.8 (16)
C1—P2—C201—C20693.7 (7)Ir1—P4—C401—C40657.0 (18)
C2—P2—C201—C20626.8 (8)C407—P4—C401—C402109.3 (17)
C207—P2—C201—C206140.8 (7)C3—P4—C401—C4027.2 (19)
C206—C201—C202—C2030.1 (12)Ir1—P4—C401—C402114.6 (17)
P2—C201—C202—C203176.1 (6)C406—C401—C402—C4035 (3)
C201—C202—C203—C2040.7 (13)P4—C401—C402—C403176.6 (16)
C202—C203—C204—C2051.8 (14)C401—C402—C403—C4043 (4)
C203—C204—C205—C2062.4 (14)C402—C403—C404—C4056 (4)
C204—C205—C206—C2011.8 (13)C403—C404—C405—C4062 (4)
C202—C201—C206—C2050.7 (12)C402—C401—C406—C40510 (3)
P2—C201—C206—C205176.5 (7)P4—C401—C406—C405178.3 (17)
C1—P2—C207—C212166.0 (5)C404—C405—C406—C4016 (3)
C2—P2—C207—C21248.1 (6)C407—P4—C41A—C42A126.6 (19)
C201—P2—C207—C21264.8 (6)C3—P4—C41A—C42A19 (2)
C1—P2—C207—C20816.9 (7)Ir1—P4—C41A—C42A101 (2)
C2—P2—C207—C208134.7 (6)C407—P4—C41A—C46A44.6 (16)
C201—P2—C207—C208112.4 (6)C3—P4—C41A—C46A152.1 (13)
C212—C207—C208—C2090.5 (10)Ir1—P4—C41A—C46A88.2 (15)
P2—C207—C208—C209177.6 (5)C46A—C41A—C42A—C43A8 (3)
C207—C208—C209—C2100.2 (10)P4—C41A—C42A—C43A179.0 (17)
C208—C209—C210—C2110.7 (12)C41A—C42A—C43A—C44A7 (3)
C209—C210—C211—C2120.6 (13)C42A—C43A—C44A—C45A3 (4)
C208—C207—C212—C2110.6 (11)C43A—C44A—C45A—C46A1 (3)
P2—C207—C212—C211177.9 (6)C44A—C45A—C46A—C41A1 (3)
C210—C211—C212—C2070.1 (12)C42A—C41A—C46A—C45A4 (3)
C1—P3—C301—C30217.1 (7)P4—C41A—C46A—C45A175.7 (16)
C3—P3—C301—C302140.7 (6)
Symmetry code: (i) x1, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2A···O5ii0.982.223.139 (15)156
C3—H3A···Cl20.982.913.693 (8)137
C3—H3B···O10.982.402.895 (10)111
C102—H102···O40.942.483.263 (11)141
C212—H212···O5ii0.942.543.445 (18)163
C306—H306···Cl20.942.573.491 (9)167
C308—H308···Cl10.942.563.464 (8)162
C408—H408···O30.942.233.046 (10)145
Symmetry code: (ii) x, y1, z.
(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}(ethoxyoxoethanylidene)methane-κ4P,C,C',P')dichloridoiridium(III) chloride–methanol–water (1/1/2) (6) top
Crystal data top
[IrCl2(C55H50O2P4)]Cl·CH4O·2H2OZ = 2
Mr = 1233.45F(000) = 1244
Triclinic, P1Dx = 1.512 Mg m3
a = 11.2371 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.9144 (2) ÅCell parameters from 58878 reflections
c = 19.2371 (3) Åθ = 1.0–25.3°
α = 89.439 (1)°µ = 2.78 mm1
β = 77.863 (1)°T = 233 K
γ = 83.114 (1)°Prism, light yellow
V = 2709.27 (8) Å30.11 × 0.05 × 0.03 mm
Data collection top
Nonius KappaCCD
diffractometer
8083 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.035
Graphite monochromatorθmax = 25.0°, θmin = 1.9°
phi– and ω–scansh = 1313
17984 measured reflectionsk = 1515
9526 independent reflectionsl = 2222
Refinement top
Refinement on F21 restraint
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.034H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.073 w = 1/[σ2(Fo2) + (0.0253P)2 + 3.0412P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.002
9526 reflectionsΔρmax = 0.75 e Å3
626 parametersΔρmin = 1.01 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Hydrogen atom at C4 found and refined isotropically with bond restraint (d = 96 pm). Hydrogens at solvent water and methanol could not be exact localized and were omitted.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ir10.20012 (2)0.37531 (2)0.74968 (2)0.02861 (6)
P10.20027 (9)0.20029 (8)0.72614 (6)0.0298 (2)
P20.46847 (9)0.22736 (8)0.70579 (6)0.0308 (2)
P30.46936 (10)0.46722 (9)0.73724 (6)0.0317 (2)
P40.20277 (10)0.55291 (8)0.76838 (6)0.0324 (2)
Cl10.01947 (9)0.39399 (9)0.79680 (6)0.0416 (3)
Cl20.16469 (10)0.43456 (9)0.63301 (5)0.0412 (3)
Cl30.44061 (18)0.83094 (12)0.72218 (9)0.0876 (5)
O10.3698 (3)0.1714 (3)0.85456 (16)0.0483 (8)
O20.2473 (3)0.2825 (2)0.93555 (14)0.0423 (7)
C10.3924 (4)0.3490 (3)0.7501 (2)0.0316 (9)
C20.3590 (4)0.1363 (3)0.7100 (2)0.0347 (10)
H2A0.36760.08700.74820.042*
H2B0.37670.09660.66510.042*
C30.3579 (4)0.5712 (3)0.7202 (2)0.0351 (10)
H3A0.35970.57380.66910.042*
H3B0.37920.63790.73480.042*
C40.3107 (4)0.3481 (3)0.8234 (2)0.0306 (9)
H40.313 (3)0.406 (2)0.8533 (16)0.021 (9)*
C50.3146 (4)0.2571 (4)0.8709 (2)0.0355 (10)
C60.2445 (5)0.2004 (4)0.9893 (2)0.0522 (13)
H6A0.32610.18230.99960.063*
H6B0.21810.13750.97210.063*
C70.1549 (5)0.2435 (4)1.0549 (2)0.0625 (15)
H7A0.15010.19161.09180.094*
H7B0.18200.30561.07120.094*
H7C0.07460.26101.04380.094*
C1010.1249 (4)0.1183 (3)0.7955 (2)0.0318 (9)
C1020.0582 (4)0.1593 (3)0.8602 (2)0.0379 (10)
H1020.04960.23170.86890.046*
C1030.0044 (4)0.0949 (4)0.9122 (2)0.0486 (12)
H1030.04080.12360.95600.058*
C1040.0168 (5)0.0112 (4)0.9002 (3)0.0498 (12)
H1040.02050.05470.93560.060*
C1050.0834 (5)0.0537 (4)0.8366 (3)0.0516 (13)
H1050.09280.12620.82860.062*
C1060.1362 (4)0.0110 (3)0.7848 (3)0.0434 (11)
H1060.18090.01810.74110.052*
C1070.1414 (4)0.1673 (3)0.6485 (2)0.0378 (10)
C1080.0346 (4)0.2249 (4)0.6382 (3)0.0497 (12)
H1080.00460.27830.67090.060*
C1090.0149 (5)0.2047 (5)0.5806 (3)0.0643 (15)
H1090.08660.24520.57360.077*
C1100.0406 (6)0.1255 (5)0.5335 (3)0.0779 (19)
H1100.00620.11090.49470.093*
C1110.1454 (7)0.0682 (5)0.5430 (3)0.088 (2)
H1110.18360.01440.51040.106*
C1120.1964 (5)0.0885 (4)0.6006 (3)0.0651 (16)
H1120.26870.04830.60680.078*
C2010.5972 (4)0.1633 (3)0.7380 (2)0.0353 (10)
C2020.6859 (4)0.2193 (4)0.7544 (2)0.0464 (12)
H2020.67630.29240.75110.056*
C2030.7880 (4)0.1694 (5)0.7753 (3)0.0574 (14)
H2030.84720.20800.78680.069*
C2040.8020 (5)0.0625 (5)0.7790 (3)0.0674 (16)
H2040.87200.02790.79250.081*
C2050.7154 (5)0.0058 (4)0.7634 (3)0.0660 (16)
H2050.72560.06720.76680.079*
C2060.6130 (4)0.0555 (4)0.7425 (3)0.0504 (12)
H2060.55410.01620.73140.061*
C2070.5223 (4)0.2456 (3)0.6120 (2)0.0345 (10)
C2080.4374 (4)0.2733 (3)0.5700 (2)0.0411 (11)
H2080.35420.29100.59120.049*
C2090.4752 (5)0.2748 (4)0.4969 (2)0.0530 (13)
H2090.41760.29300.46850.064*
C2100.5969 (5)0.2499 (4)0.4655 (3)0.0602 (14)
H2100.62200.25060.41580.072*
C2110.6822 (5)0.2238 (4)0.5066 (3)0.0619 (15)
H2110.76560.20850.48490.074*
C2120.6456 (4)0.2203 (4)0.5801 (2)0.0470 (12)
H2120.70360.20090.60810.056*
C3010.6002 (4)0.4688 (3)0.6643 (2)0.0342 (10)
C3020.5845 (4)0.4801 (3)0.5945 (2)0.0401 (11)
H3020.50550.48280.58490.048*
C3030.6836 (4)0.4873 (4)0.5395 (3)0.0511 (13)
H3030.67250.49450.49250.061*
C3040.7992 (5)0.4838 (4)0.5537 (3)0.0596 (14)
H3040.86670.48880.51600.072*
C3050.8176 (4)0.4733 (4)0.6219 (3)0.0570 (14)
H3050.89710.47040.63070.068*
C3060.7178 (4)0.4669 (4)0.6779 (2)0.0430 (11)
H3060.72950.46140.72480.052*
C3070.5217 (4)0.4991 (4)0.8154 (2)0.0411 (11)
C3080.5459 (4)0.4239 (4)0.8648 (2)0.0504 (13)
H3080.52780.35550.86010.060*
C3090.5969 (5)0.4504 (5)0.9211 (3)0.0668 (16)
H3090.61500.39970.95400.080*
C3100.6206 (6)0.5507 (6)0.9284 (3)0.082 (2)
H3100.65440.56840.96680.098*
C3110.5960 (6)0.6261 (5)0.8810 (3)0.0756 (18)
H3110.61190.69480.88740.091*
C3120.5475 (5)0.6009 (4)0.8232 (3)0.0577 (14)
H3120.53230.65190.78990.069*
C4010.1033 (4)0.6511 (3)0.7316 (2)0.0416 (11)
C4020.0197 (5)0.6456 (5)0.7435 (4)0.085 (2)
H4020.05310.59180.77140.103*
C4030.0963 (6)0.7187 (5)0.7150 (5)0.105 (3)
H4030.18040.71230.72210.126*
C4040.0511 (7)0.7988 (5)0.6771 (3)0.0805 (19)
H4040.10320.84690.65690.097*
C4050.0713 (7)0.8101 (4)0.6681 (3)0.0760 (19)
H4050.10230.86730.64310.091*
C4060.1491 (5)0.7372 (4)0.6958 (3)0.0628 (15)
H4060.23240.74580.69060.075*
C4070.1915 (4)0.5998 (3)0.8588 (2)0.0380 (10)
C4080.1376 (4)0.5429 (4)0.9163 (2)0.0441 (11)
H4080.10690.48050.90820.053*
C4090.1289 (4)0.5774 (4)0.9851 (3)0.0510 (13)
H4090.09320.53821.02360.061*
C4100.1727 (4)0.6695 (4)0.9971 (3)0.0531 (13)
H4100.16680.69321.04390.064*
C4110.2245 (4)0.7260 (4)0.9410 (3)0.0520 (13)
H4110.25350.78900.94940.062*
C4120.2349 (4)0.6920 (4)0.8722 (2)0.0442 (11)
H4120.27150.73160.83410.053*
C80.3855 (8)0.1059 (8)1.0516 (4)0.124 (3)
O30.4612 (6)0.1618 (6)0.9936 (4)0.156 (3)
O40.3991 (6)0.0653 (4)0.8766 (3)0.127 (2)
O50.5148 (8)0.9672 (4)0.5852 (4)0.171 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.02499 (9)0.03004 (10)0.03009 (10)0.00432 (6)0.00380 (6)0.00424 (6)
P10.0260 (6)0.0305 (6)0.0336 (6)0.0062 (5)0.0062 (5)0.0035 (5)
P20.0254 (6)0.0334 (6)0.0328 (6)0.0032 (5)0.0043 (4)0.0021 (5)
P30.0293 (6)0.0358 (6)0.0300 (6)0.0091 (5)0.0036 (5)0.0019 (5)
P40.0310 (6)0.0299 (6)0.0332 (6)0.0039 (5)0.0000 (5)0.0030 (5)
Cl10.0270 (5)0.0447 (7)0.0494 (7)0.0032 (5)0.0003 (5)0.0070 (5)
Cl20.0394 (6)0.0490 (7)0.0335 (6)0.0004 (5)0.0074 (5)0.0092 (5)
Cl30.1165 (14)0.0610 (10)0.0883 (11)0.0425 (10)0.0108 (10)0.0024 (8)
O10.048 (2)0.044 (2)0.0483 (19)0.0049 (16)0.0053 (15)0.0074 (15)
O20.0508 (19)0.0459 (19)0.0287 (16)0.0077 (15)0.0043 (14)0.0107 (13)
C10.030 (2)0.030 (2)0.034 (2)0.0041 (18)0.0044 (18)0.0008 (18)
C20.030 (2)0.033 (2)0.040 (2)0.0042 (19)0.0038 (19)0.0006 (19)
C30.038 (2)0.029 (2)0.036 (2)0.0079 (19)0.0013 (19)0.0037 (18)
C40.032 (2)0.034 (2)0.027 (2)0.0089 (19)0.0041 (18)0.0009 (18)
C50.029 (2)0.046 (3)0.034 (2)0.009 (2)0.0101 (19)0.003 (2)
C60.058 (3)0.061 (3)0.039 (3)0.011 (3)0.011 (2)0.023 (2)
C70.076 (4)0.075 (4)0.039 (3)0.028 (3)0.006 (3)0.012 (3)
C1010.025 (2)0.030 (2)0.042 (2)0.0065 (18)0.0106 (19)0.0082 (19)
C1020.036 (2)0.038 (3)0.040 (3)0.004 (2)0.010 (2)0.004 (2)
C1030.052 (3)0.054 (3)0.040 (3)0.013 (2)0.007 (2)0.011 (2)
C1040.053 (3)0.053 (3)0.046 (3)0.015 (3)0.013 (2)0.022 (2)
C1050.058 (3)0.035 (3)0.061 (3)0.007 (2)0.009 (3)0.015 (2)
C1060.041 (3)0.036 (3)0.050 (3)0.002 (2)0.003 (2)0.006 (2)
C1070.039 (3)0.038 (3)0.040 (2)0.011 (2)0.012 (2)0.003 (2)
C1080.037 (3)0.062 (3)0.052 (3)0.005 (2)0.015 (2)0.002 (2)
C1090.053 (3)0.079 (4)0.070 (4)0.006 (3)0.034 (3)0.004 (3)
C1100.095 (5)0.077 (4)0.078 (4)0.010 (4)0.056 (4)0.009 (4)
C1110.120 (6)0.070 (4)0.086 (5)0.010 (4)0.060 (4)0.038 (4)
C1120.082 (4)0.051 (3)0.069 (4)0.010 (3)0.039 (3)0.017 (3)
C2010.030 (2)0.038 (3)0.034 (2)0.002 (2)0.0022 (18)0.0012 (19)
C2020.040 (3)0.047 (3)0.056 (3)0.014 (2)0.016 (2)0.010 (2)
C2030.037 (3)0.073 (4)0.068 (3)0.007 (3)0.025 (3)0.012 (3)
C2040.041 (3)0.076 (4)0.086 (4)0.009 (3)0.028 (3)0.021 (3)
C2050.051 (3)0.044 (3)0.104 (5)0.008 (3)0.025 (3)0.007 (3)
C2060.034 (3)0.042 (3)0.077 (4)0.002 (2)0.016 (2)0.000 (2)
C2070.034 (2)0.033 (2)0.034 (2)0.0073 (19)0.0010 (19)0.0009 (18)
C2080.040 (3)0.041 (3)0.041 (3)0.005 (2)0.006 (2)0.002 (2)
C2090.062 (3)0.060 (3)0.038 (3)0.003 (3)0.014 (2)0.007 (2)
C2100.069 (4)0.070 (4)0.035 (3)0.001 (3)0.001 (3)0.003 (3)
C2110.046 (3)0.082 (4)0.047 (3)0.001 (3)0.009 (3)0.001 (3)
C2120.033 (3)0.060 (3)0.044 (3)0.004 (2)0.001 (2)0.001 (2)
C3010.029 (2)0.034 (2)0.038 (2)0.0064 (19)0.0035 (19)0.0058 (19)
C3020.034 (2)0.047 (3)0.036 (3)0.006 (2)0.0008 (19)0.006 (2)
C3030.047 (3)0.060 (3)0.039 (3)0.003 (2)0.001 (2)0.010 (2)
C3040.042 (3)0.073 (4)0.051 (3)0.000 (3)0.013 (2)0.009 (3)
C3050.028 (3)0.067 (4)0.070 (4)0.007 (2)0.002 (2)0.013 (3)
C3060.033 (2)0.050 (3)0.049 (3)0.013 (2)0.011 (2)0.012 (2)
C3070.032 (2)0.052 (3)0.039 (3)0.013 (2)0.003 (2)0.006 (2)
C3080.045 (3)0.071 (4)0.039 (3)0.021 (3)0.011 (2)0.002 (2)
C3090.055 (3)0.111 (5)0.041 (3)0.025 (3)0.019 (3)0.011 (3)
C3100.077 (4)0.126 (6)0.052 (4)0.040 (4)0.021 (3)0.014 (4)
C3110.076 (4)0.083 (5)0.079 (4)0.036 (4)0.026 (3)0.021 (4)
C3120.056 (3)0.060 (3)0.059 (3)0.017 (3)0.012 (3)0.011 (3)
C4010.046 (3)0.035 (3)0.040 (3)0.003 (2)0.005 (2)0.003 (2)
C4020.047 (3)0.053 (4)0.157 (7)0.003 (3)0.027 (4)0.045 (4)
C4030.061 (4)0.060 (4)0.197 (9)0.000 (3)0.041 (5)0.035 (5)
C4040.084 (5)0.065 (4)0.086 (5)0.031 (4)0.025 (4)0.011 (3)
C4050.099 (5)0.050 (4)0.064 (4)0.014 (3)0.001 (3)0.022 (3)
C4060.068 (4)0.051 (3)0.060 (3)0.000 (3)0.004 (3)0.013 (3)
C4070.036 (2)0.036 (3)0.040 (3)0.005 (2)0.001 (2)0.002 (2)
C4080.046 (3)0.041 (3)0.040 (3)0.009 (2)0.003 (2)0.001 (2)
C4090.047 (3)0.056 (3)0.044 (3)0.009 (3)0.006 (2)0.004 (2)
C4100.048 (3)0.065 (4)0.041 (3)0.002 (3)0.001 (2)0.009 (3)
C4110.051 (3)0.050 (3)0.055 (3)0.011 (2)0.006 (2)0.013 (3)
C4120.044 (3)0.041 (3)0.044 (3)0.007 (2)0.000 (2)0.001 (2)
C80.114 (7)0.164 (9)0.085 (6)0.000 (6)0.011 (5)0.033 (6)
O30.119 (5)0.197 (7)0.158 (6)0.022 (5)0.060 (4)0.045 (5)
O40.188 (6)0.105 (4)0.098 (4)0.055 (4)0.035 (4)0.022 (3)
O50.305 (10)0.074 (4)0.157 (6)0.004 (5)0.112 (6)0.028 (4)
Geometric parameters (Å, º) top
Ir1—C42.076 (4)C203—H2030.9400
Ir1—C12.149 (4)C204—C2051.369 (7)
Ir1—P12.3093 (11)C204—H2040.9400
Ir1—P42.3298 (11)C205—C2061.381 (7)
Ir1—Cl12.4268 (10)C205—H2050.9400
Ir1—Cl22.4597 (10)C206—H2060.9400
P1—C1011.825 (4)C207—C2081.389 (6)
P1—C1071.830 (4)C207—C2121.394 (6)
P1—C21.838 (4)C208—C2091.382 (6)
P2—C21.790 (4)C208—H2080.9400
P2—C2071.800 (4)C209—C2101.374 (7)
P2—C2011.801 (4)C209—H2090.9400
P2—C11.822 (4)C210—C2111.376 (7)
P3—C3071.793 (4)C210—H2100.9400
P3—C31.800 (4)C211—C2121.389 (6)
P3—C3011.809 (4)C211—H2110.9400
P3—C11.833 (4)C212—H2120.9400
P4—C4071.821 (4)C301—C3021.395 (6)
P4—C4011.825 (4)C301—C3061.397 (6)
P4—C31.835 (4)C302—C3031.378 (6)
O1—C51.213 (5)C302—H3020.9400
O2—C51.333 (5)C303—C3041.378 (7)
O2—C61.472 (5)C303—H3030.9400
C1—C41.513 (5)C304—C3051.373 (7)
C2—H2A0.9800C304—H3040.9400
C2—H2B0.9800C305—C3061.392 (6)
C3—H3A0.9800C305—H3050.9400
C3—H3B0.9800C306—H3060.9400
C4—C51.483 (6)C307—C3081.396 (7)
C4—H40.954 (18)C307—C3121.397 (7)
C6—C71.504 (7)C308—C3091.391 (7)
C6—H6A0.9800C308—H3080.9400
C6—H6B0.9800C309—C3101.368 (9)
C7—H7A0.9700C309—H3090.9400
C7—H7B0.9700C310—C3111.371 (9)
C7—H7C0.9700C310—H3100.9400
C101—C1021.385 (6)C311—C3121.394 (7)
C101—C1061.389 (6)C311—H3110.9400
C102—C1031.382 (6)C312—H3120.9400
C102—H1020.9400C401—C4021.364 (7)
C103—C1041.379 (7)C401—C4061.396 (7)
C103—H1030.9400C402—C4031.388 (8)
C104—C1051.373 (7)C402—H4020.9400
C104—H1040.9400C403—C4041.346 (9)
C105—C1061.378 (6)C403—H4030.9400
C105—H1050.9400C404—C4051.375 (9)
C106—H1060.9400C404—H4040.9400
C107—C1121.376 (7)C405—C4061.387 (8)
C107—C1081.383 (6)C405—H4050.9400
C108—C1091.381 (7)C406—H4060.9400
C108—H1080.9400C407—C4121.386 (6)
C109—C1101.373 (8)C407—C4081.393 (6)
C109—H1090.9400C408—C4091.380 (6)
C110—C1111.358 (8)C408—H4080.9400
C110—H1100.9400C409—C4101.380 (7)
C111—C1121.391 (7)C409—H4090.9400
C111—H1110.9400C410—C4111.364 (7)
C112—H1120.9400C410—H4100.9400
C201—C2061.386 (6)C411—C4121.376 (6)
C201—C2021.387 (6)C411—H4110.9400
C202—C2031.381 (6)C412—H4120.9400
C202—H2020.9400C8—O31.400 (9)
C203—C2041.373 (8)
C4—Ir1—C141.94 (15)C107—C112—C111120.2 (5)
C4—Ir1—P193.94 (12)C107—C112—H112119.9
C1—Ir1—P190.24 (11)C111—C112—H112119.9
C4—Ir1—P487.46 (12)C206—C201—C202118.8 (4)
C1—Ir1—P489.52 (11)C206—C201—P2119.9 (3)
P1—Ir1—P4177.61 (4)C202—C201—P2121.1 (3)
C4—Ir1—Cl1116.21 (11)C203—C202—C201121.0 (5)
C1—Ir1—Cl1158.13 (11)C203—C202—H202119.5
P1—Ir1—Cl190.79 (4)C201—C202—H202119.5
P4—Ir1—Cl190.32 (4)C204—C203—C202119.1 (5)
C4—Ir1—Cl2151.91 (11)C204—C203—H203120.5
C1—Ir1—Cl2111.50 (11)C202—C203—H203120.5
P1—Ir1—Cl295.28 (4)C205—C204—C203120.8 (5)
P4—Ir1—Cl282.61 (4)C205—C204—H204119.6
Cl1—Ir1—Cl290.15 (4)C203—C204—H204119.6
C101—P1—C107103.22 (19)C204—C205—C206120.3 (5)
C101—P1—C2101.10 (19)C204—C205—H205119.9
C107—P1—C2105.4 (2)C206—C205—H205119.9
C101—P1—Ir1119.47 (14)C205—C206—C201120.0 (5)
C107—P1—Ir1116.96 (15)C205—C206—H206120.0
C2—P1—Ir1108.79 (13)C201—C206—H206120.0
C2—P2—C207104.15 (19)C208—C207—C212119.6 (4)
C2—P2—C201107.7 (2)C208—C207—P2119.1 (3)
C207—P2—C201106.31 (19)C212—C207—P2120.8 (3)
C2—P2—C1109.35 (19)C209—C208—C207120.0 (4)
C207—P2—C1111.24 (19)C209—C208—H208120.0
C201—P2—C1117.21 (19)C207—C208—H208120.0
C307—P3—C3109.2 (2)C210—C209—C208120.2 (5)
C307—P3—C301105.7 (2)C210—C209—H209119.9
C3—P3—C301105.53 (19)C208—C209—H209119.9
C307—P3—C1111.0 (2)C209—C210—C211120.4 (5)
C3—P3—C1106.85 (19)C209—C210—H210119.8
C301—P3—C1118.24 (19)C211—C210—H210119.8
C407—P4—C401103.8 (2)C210—C211—C212120.2 (5)
C407—P4—C3105.7 (2)C210—C211—H211119.9
C401—P4—C3104.1 (2)C212—C211—H211119.9
C407—P4—Ir1118.43 (14)C211—C212—C207119.5 (5)
C401—P4—Ir1121.43 (15)C211—C212—H212120.2
C3—P4—Ir1101.43 (14)C207—C212—H212120.2
C5—O2—C6116.4 (4)C302—C301—C306119.1 (4)
C4—C1—P2120.5 (3)C302—C301—P3120.6 (3)
C4—C1—P3111.2 (3)C306—C301—P3120.1 (3)
P2—C1—P3119.9 (2)C303—C302—C301120.5 (4)
C4—C1—Ir166.5 (2)C303—C302—H302119.7
P2—C1—Ir1113.31 (19)C301—C302—H302119.7
P3—C1—Ir1113.9 (2)C302—C303—C304119.7 (5)
P2—C2—P1112.6 (2)C302—C303—H303120.2
P2—C2—H2A109.1C304—C303—H303120.2
P1—C2—H2A109.1C305—C304—C303121.2 (4)
P2—C2—H2B109.1C305—C304—H304119.4
P1—C2—H2B109.1C303—C304—H304119.4
H2A—C2—H2B107.8C304—C305—C306119.6 (5)
P3—C3—P4111.4 (2)C304—C305—H305120.2
P3—C3—H3A109.3C306—C305—H305120.2
P4—C3—H3A109.3C305—C306—C301119.9 (4)
P3—C3—H3B109.3C305—C306—H306120.1
P4—C3—H3B109.3C301—C306—H306120.1
H3A—C3—H3B108.0C308—C307—C312119.7 (4)
C5—C4—C1122.7 (4)C308—C307—P3122.1 (4)
C5—C4—Ir1126.2 (3)C312—C307—P3118.0 (4)
C1—C4—Ir171.6 (2)C309—C308—C307120.0 (5)
C5—C4—H4104 (2)C309—C308—H308120.0
C1—C4—H4115 (2)C307—C308—H308120.0
Ir1—C4—H4116 (2)C310—C309—C308119.6 (6)
O1—C5—O2123.9 (4)C310—C309—H309120.2
O1—C5—C4126.0 (4)C308—C309—H309120.2
O2—C5—C4110.1 (4)C309—C310—C311121.4 (5)
O2—C6—C7106.7 (4)C309—C310—H310119.3
O2—C6—H6A110.4C311—C310—H310119.3
C7—C6—H6A110.4C310—C311—C312120.1 (6)
O2—C6—H6B110.4C310—C311—H311120.0
C7—C6—H6B110.4C312—C311—H311120.0
H6A—C6—H6B108.6C311—C312—C307119.2 (5)
C6—C7—H7A109.5C311—C312—H312120.4
C6—C7—H7B109.5C307—C312—H312120.4
H7A—C7—H7B109.5C402—C401—C406118.5 (5)
C6—C7—H7C109.5C402—C401—P4120.1 (4)
H7A—C7—H7C109.5C406—C401—P4121.2 (4)
H7B—C7—H7C109.5C401—C402—C403120.8 (6)
C102—C101—C106118.1 (4)C401—C402—H402119.6
C102—C101—P1122.0 (3)C403—C402—H402119.6
C106—C101—P1119.9 (3)C404—C403—C402120.6 (6)
C103—C102—C101120.6 (4)C404—C403—H403119.7
C103—C102—H102119.7C402—C403—H403119.7
C101—C102—H102119.7C403—C404—C405119.9 (6)
C104—C103—C102120.1 (5)C403—C404—H404120.1
C104—C103—H103119.9C405—C404—H404120.1
C102—C103—H103119.9C404—C405—C406120.2 (6)
C105—C104—C103120.2 (4)C404—C405—H405119.9
C105—C104—H104119.9C406—C405—H405119.9
C103—C104—H104119.9C405—C406—C401119.8 (6)
C104—C105—C106119.3 (5)C405—C406—H406120.1
C104—C105—H105120.3C401—C406—H406120.1
C106—C105—H105120.3C412—C407—C408118.6 (4)
C105—C106—C101121.6 (4)C412—C407—P4121.5 (3)
C105—C106—H106119.2C408—C407—P4120.0 (3)
C101—C106—H106119.2C409—C408—C407120.5 (4)
C112—C107—C108118.7 (4)C409—C408—H408119.7
C112—C107—P1123.8 (4)C407—C408—H408119.7
C108—C107—P1117.5 (3)C408—C409—C410119.9 (5)
C109—C108—C107120.7 (5)C408—C409—H409120.1
C109—C108—H108119.7C410—C409—H409120.1
C107—C108—H108119.7C411—C410—C409119.9 (5)
C110—C109—C108120.0 (5)C411—C410—H410120.1
C110—C109—H109120.0C409—C410—H410120.1
C108—C109—H109120.0C410—C411—C412120.9 (5)
C111—C110—C109119.9 (5)C410—C411—H411119.6
C111—C110—H110120.0C412—C411—H411119.6
C109—C110—H110120.0C411—C412—C407120.3 (4)
C110—C111—C112120.5 (6)C411—C412—H412119.9
C110—C111—H111119.8C407—C412—H412119.9
C112—C111—H111119.8
C2—P2—C1—C448.9 (4)P2—C201—C202—C203176.4 (4)
C207—P2—C1—C4163.4 (3)C201—C202—C203—C2040.8 (8)
C201—P2—C1—C474.0 (4)C202—C203—C204—C2051.0 (9)
C2—P2—C1—P3165.7 (2)C203—C204—C205—C2061.0 (9)
C207—P2—C1—P351.2 (3)C204—C205—C206—C2010.6 (9)
C201—P2—C1—P371.4 (3)C202—C201—C206—C2050.4 (7)
C2—P2—C1—Ir126.5 (3)P2—C201—C206—C205176.3 (4)
C207—P2—C1—Ir188.0 (2)C2—P2—C207—C20853.0 (4)
C201—P2—C1—Ir1149.5 (2)C201—P2—C207—C208166.7 (3)
C307—P3—C1—C441.4 (3)C1—P2—C207—C20864.7 (4)
C3—P3—C1—C477.6 (3)C2—P2—C207—C212119.3 (4)
C301—P3—C1—C4163.7 (3)C201—P2—C207—C2125.6 (4)
C307—P3—C1—P2107.0 (3)C1—P2—C207—C212123.0 (4)
C3—P3—C1—P2134.1 (2)C212—C207—C208—C2090.6 (7)
C301—P3—C1—P215.4 (3)P2—C207—C208—C209171.8 (4)
C307—P3—C1—Ir1114.1 (2)C207—C208—C209—C2100.6 (7)
C3—P3—C1—Ir14.9 (3)C208—C209—C210—C2110.5 (8)
C301—P3—C1—Ir1123.6 (2)C209—C210—C211—C2121.5 (9)
C207—P2—C2—P198.2 (2)C210—C211—C212—C2071.5 (8)
C201—P2—C2—P1149.2 (2)C208—C207—C212—C2110.5 (7)
C1—P2—C2—P120.8 (3)P2—C207—C212—C211172.7 (4)
C101—P1—C2—P2133.9 (2)C307—P3—C301—C302159.6 (4)
C107—P1—C2—P2118.9 (2)C3—P3—C301—C30244.0 (4)
Ir1—P1—C2—P27.3 (3)C1—P3—C301—C30275.4 (4)
C307—P3—C3—P487.5 (3)C307—P3—C301—C30615.4 (4)
C301—P3—C3—P4159.3 (2)C3—P3—C301—C306131.0 (4)
C1—P3—C3—P432.7 (3)C1—P3—C301—C306109.6 (4)
C407—P4—C3—P381.0 (3)C306—C301—C302—C3031.2 (7)
C401—P4—C3—P3170.0 (2)P3—C301—C302—C303176.2 (4)
Ir1—P4—C3—P343.2 (2)C301—C302—C303—C3040.3 (7)
P2—C1—C4—C517.6 (5)C302—C303—C304—C3050.0 (8)
P3—C1—C4—C5130.5 (3)C303—C304—C305—C3060.6 (8)
Ir1—C1—C4—C5121.8 (4)C304—C305—C306—C3011.5 (8)
P2—C1—C4—Ir1104.1 (3)C302—C301—C306—C3051.8 (7)
P3—C1—C4—Ir1107.8 (2)P3—C301—C306—C305176.9 (4)
C6—O2—C5—O11.6 (6)C3—P3—C307—C308141.9 (4)
C6—O2—C5—C4178.7 (3)C301—P3—C307—C308105.0 (4)
C1—C4—C5—O19.5 (6)C1—P3—C307—C30824.3 (4)
Ir1—C4—C5—O180.8 (5)C3—P3—C307—C31243.2 (4)
C1—C4—C5—O2170.8 (3)C301—P3—C307—C31269.9 (4)
Ir1—C4—C5—O298.9 (4)C1—P3—C307—C312160.7 (4)
C5—O2—C6—C7174.9 (4)C312—C307—C308—C3090.7 (7)
C107—P1—C101—C102126.3 (3)P3—C307—C308—C309174.1 (4)
C2—P1—C101—C102124.8 (3)C307—C308—C309—C3101.3 (8)
Ir1—P1—C101—C1025.6 (4)C308—C309—C310—C3110.5 (10)
C107—P1—C101—C10655.4 (4)C309—C310—C311—C3120.9 (10)
C2—P1—C101—C10653.5 (4)C310—C311—C312—C3071.6 (9)
Ir1—P1—C101—C106172.7 (3)C308—C307—C312—C3110.7 (7)
C106—C101—C102—C1030.3 (6)P3—C307—C312—C311175.8 (4)
P1—C101—C102—C103178.6 (3)C407—P4—C401—C40284.0 (5)
C101—C102—C103—C1040.2 (7)C3—P4—C401—C402165.6 (5)
C102—C103—C104—C1050.4 (7)Ir1—P4—C401—C40252.5 (5)
C103—C104—C105—C1060.9 (7)C407—P4—C401—C40690.9 (4)
C104—C105—C106—C1010.7 (7)C3—P4—C401—C40619.6 (4)
C102—C101—C106—C1050.1 (6)Ir1—P4—C401—C406132.7 (4)
P1—C101—C106—C105178.2 (4)C406—C401—C402—C4036.0 (10)
C101—P1—C107—C11289.9 (5)P4—C401—C402—C403178.9 (6)
C2—P1—C107—C11215.7 (5)C401—C402—C403—C4042.5 (12)
Ir1—P1—C107—C112136.7 (4)C402—C403—C404—C4051.7 (12)
C101—P1—C107—C10889.5 (4)C403—C404—C405—C4062.2 (10)
C2—P1—C107—C108164.9 (4)C404—C405—C406—C4011.4 (9)
Ir1—P1—C107—C10843.8 (4)C402—C401—C406—C4055.5 (8)
C112—C107—C108—C1090.9 (8)P4—C401—C406—C405179.6 (4)
P1—C107—C108—C109179.7 (4)C401—P4—C407—C41265.3 (4)
C107—C108—C109—C1101.3 (9)C3—P4—C407—C41243.9 (4)
C108—C109—C110—C1111.1 (10)Ir1—P4—C407—C412156.7 (3)
C109—C110—C111—C1120.6 (11)C401—P4—C407—C408114.3 (4)
C108—C107—C112—C1110.4 (8)C3—P4—C407—C408136.5 (4)
P1—C107—C112—C111179.8 (5)Ir1—P4—C407—C40823.8 (4)
C110—C111—C112—C1070.3 (11)C412—C407—C408—C4090.7 (7)
C2—P2—C201—C20616.9 (4)P4—C407—C408—C409179.8 (4)
C207—P2—C201—C20694.3 (4)C407—C408—C409—C4100.7 (7)
C1—P2—C201—C206140.7 (4)C408—C409—C410—C4110.1 (8)
C2—P2—C201—C202167.2 (4)C409—C410—C411—C4120.6 (8)
C207—P2—C201—C20281.6 (4)C410—C411—C412—C4070.6 (7)
C1—P2—C201—C20243.5 (4)C408—C407—C412—C4110.0 (7)
C206—C201—C202—C2030.4 (7)P4—C407—C412—C411179.6 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2A···O10.982.332.852 (5)112
C2—H2B···O5i0.982.453.320 (8)148
C3—H3B···Cl30.982.663.589 (4)158
C6—H6A···O3ii0.982.403.369 (8)169
C102—H102···Cl10.942.633.343 (4)133
C108—H108···Cl10.942.823.671 (5)151
C206—H206···Cl3i0.942.873.742 (5)156
C208—H208···Cl20.942.643.487 (5)150
C312—H312···Cl30.942.843.749 (6)164
C402—H402···Cl10.942.593.398 (6)144
C406—H406···Cl30.942.883.757 (6)156
C412—H412···Cl30.942.953.870 (5)167
Symmetry codes: (i) x, y1, z; (ii) x+1, y, z+2.
(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}(ethoxyoxoethanylidene)methane-κ4P,C,C',P')carbonyl(ethoxyoxoethanide)iridium(III) dichloride–methylene chloride–water (1/2/1.5) (7) top
Crystal data top
[Ir(C4H7O2)(C55H50O2P4)(CO)]Cl2·2CH2Cl2·1.5H2OZ = 2
Mr = 1441.91F(000) = 1454
Triclinic, P1Dx = 1.505 Mg m3
a = 11.7326 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.8815 (2) ÅCell parameters from 109564 reflections
c = 22.2615 (3) Åθ = 1.0–27.4°
α = 75.477 (1)°µ = 2.50 mm1
β = 86.508 (1)°T = 233 K
γ = 65.212 (1)°Prism, yellow
V = 3182.38 (9) Å30.31 × 0.23 × 0.19 mm
Data collection top
Nonius KappaCCD
diffractometer
11695 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.024
Graphite monochromatorθmax = 26.0°, θmin = 1.9°
phi– and ω–scansh = 1414
23329 measured reflectionsk = 1716
12496 independent reflectionsl = 2627
Refinement top
Refinement on F23 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.070 w = 1/[σ2(Fo2) + (0.026P)2 + 5.2527P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
12496 reflectionsΔρmax = 0.97 e Å3
751 parametersΔρmin = 1.29 e Å3
Special details top

Experimental. All data sets were measured with several scans to increase the number of redundant reflections. In our experience this method of averaging redundant reflections replaces in a good approximation semi-empirical absorptions methods (absorption correction programs like SORTAV lead to no better data sets).

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Hydrogen at C4 was found and refined isotropically with bond restraint (d=96pm). Hydrogens at water O6 were found and refined isotropically with bond restraints (d=84pm). The water molecule O7 was half occupied and hydrogen of it were omitted. The chlorine atoms at solvent dichloromethane CL5-C14-Cl6 were positional disordered in ratio around 2:1 (CL5-6: Cl5A-6A). C14=C14A with equal coordinates and displacement parameters for hydrogen calculation.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ir10.18100 (2)0.32675 (2)0.19059 (2)0.02360 (4)
P10.01647 (7)0.32287 (7)0.20407 (4)0.02798 (16)
P20.08519 (8)0.24968 (7)0.33707 (4)0.02951 (17)
P30.36173 (7)0.23582 (6)0.31877 (3)0.02553 (16)
P40.38428 (7)0.32406 (6)0.18358 (3)0.02485 (15)
O10.2405 (2)0.4989 (2)0.30318 (12)0.0441 (6)
O20.0747 (2)0.60098 (18)0.23599 (11)0.0398 (6)
O30.2584 (3)0.4317 (3)0.02412 (12)0.0555 (7)
O40.1299 (3)0.3486 (2)0.02816 (11)0.0512 (7)
O50.2606 (3)0.1321 (2)0.13439 (14)0.0542 (7)
C10.1994 (3)0.2948 (2)0.29337 (13)0.0258 (6)
C20.0016 (3)0.2266 (3)0.28035 (14)0.0322 (7)
H2A0.08160.23490.29500.039*
H2B0.04750.15150.27610.039*
C30.4342 (3)0.3087 (3)0.26346 (13)0.0275 (6)
H3A0.52590.26880.26900.033*
H3B0.41090.38130.27070.033*
C40.1312 (3)0.4148 (2)0.26037 (13)0.0264 (6)
H40.0434 (18)0.441 (3)0.2635 (15)0.030 (9)*
C50.1589 (3)0.5053 (3)0.26978 (15)0.0320 (7)
C60.0842 (4)0.7004 (3)0.2418 (2)0.0530 (10)
H6A0.17020.69390.23510.064*
H6B0.06180.71230.28330.064*
C70.0043 (6)0.7923 (4)0.1938 (3)0.093 (2)
H7A0.00110.86010.19600.140*
H7B0.01900.77950.15300.140*
H7C0.08890.79770.20100.140*
C80.1075 (3)0.4468 (3)0.10236 (14)0.0334 (7)
H8A0.01840.46330.09670.040*
H8B0.11270.51470.10410.040*
C90.1736 (3)0.4113 (3)0.04821 (14)0.0368 (7)
C100.1946 (5)0.3027 (4)0.0222 (2)0.0668 (13)
H10A0.28290.25430.00950.080*
H10B0.19160.36120.05840.080*
C110.1298 (7)0.2398 (5)0.0379 (3)0.099 (2)
H11A0.17080.20760.07170.149*
H11B0.13350.18210.00180.149*
H11C0.04260.28850.05050.149*
C120.2317 (3)0.2051 (3)0.15415 (15)0.0331 (7)
C1010.0676 (3)0.2706 (3)0.14917 (15)0.0335 (7)
C1020.0305 (4)0.1594 (3)0.15564 (19)0.0524 (10)
H1020.01930.10790.19060.063*
C1030.0678 (5)0.1250 (4)0.1099 (2)0.0660 (13)
H1030.04430.04980.11440.079*
C1040.1382 (5)0.1990 (4)0.0586 (2)0.0607 (12)
H1040.16250.17430.02800.073*
C1050.1736 (4)0.3080 (4)0.05112 (18)0.0506 (10)
H1050.22190.35830.01550.061*
C1060.1383 (3)0.3449 (3)0.09598 (16)0.0416 (8)
H1060.16220.42030.09060.050*
C1070.1551 (3)0.4470 (3)0.20753 (15)0.0343 (7)
C1080.1557 (3)0.5505 (3)0.19268 (16)0.0397 (8)
H1080.08190.55880.17980.048*
C1090.2639 (4)0.6416 (3)0.1967 (2)0.0544 (10)
H1090.26360.71140.18690.065*
C1100.3727 (4)0.6289 (4)0.2153 (2)0.0639 (12)
H1100.44630.69030.21860.077*
C1110.3735 (4)0.5262 (4)0.2292 (2)0.0586 (11)
H1110.44780.51830.24160.070*
C1120.2664 (3)0.4361 (3)0.22511 (17)0.0454 (9)
H1120.26780.36670.23410.055*
C2010.1375 (3)0.1290 (3)0.40066 (14)0.0360 (7)
C2020.1785 (4)0.0254 (3)0.39114 (18)0.0494 (9)
H2020.18380.01620.35050.059*
C2030.2117 (5)0.0648 (4)0.4412 (2)0.0710 (14)
H2030.24090.13520.43440.085*
C2040.2025 (5)0.0524 (4)0.5010 (2)0.0754 (15)
H2040.22550.11420.53480.091*
C2050.1602 (5)0.0495 (4)0.51097 (19)0.0699 (14)
H2050.15360.05760.55190.084*
C2060.1266 (4)0.1415 (4)0.46165 (17)0.0538 (10)
H2060.09680.21160.46900.065*
C2070.0190 (3)0.3598 (3)0.36982 (15)0.0404 (8)
C2080.0283 (4)0.4210 (4)0.39200 (18)0.0542 (10)
H2080.11430.40530.38960.065*
C2090.0505 (6)0.5050 (5)0.4177 (2)0.0834 (17)
H2090.01800.54650.43270.100*
C2100.1743 (7)0.5277 (6)0.4213 (3)0.100 (2)
H2100.22800.58600.43790.121*
C2110.2220 (5)0.4656 (6)0.4006 (3)0.100 (2)
H2110.30780.48110.40430.119*
C2120.1449 (4)0.3800 (4)0.37442 (19)0.0615 (12)
H2120.17730.33750.36040.074*
C3010.3972 (3)0.2405 (3)0.39562 (14)0.0319 (7)
C3020.3965 (4)0.1578 (3)0.44585 (16)0.0452 (9)
H3020.37750.10160.43940.054*
C3030.4237 (5)0.1584 (4)0.50518 (18)0.0617 (12)
H3030.42150.10330.53920.074*
C3040.4536 (5)0.2385 (4)0.51477 (18)0.0635 (13)
H3040.47230.23780.55540.076*
C3050.4568 (4)0.3201 (4)0.46571 (19)0.0589 (11)
H3050.47810.37470.47270.071*
C3060.4285 (4)0.3214 (3)0.40556 (17)0.0444 (9)
H3060.43050.37700.37180.053*
C3070.4396 (3)0.0935 (2)0.31728 (14)0.0294 (6)
C3080.3872 (3)0.0411 (3)0.28949 (16)0.0382 (8)
H3080.30390.07850.27280.046*
C3090.4580 (4)0.0664 (3)0.28642 (19)0.0503 (9)
H3090.42170.10230.26860.060*
C3100.5809 (4)0.1206 (3)0.3093 (2)0.0522 (10)
H3100.62870.19300.30630.063*
C3110.6345 (4)0.0693 (3)0.33646 (18)0.0451 (9)
H3110.71870.10650.35170.054*
C3120.5640 (3)0.0370 (3)0.34124 (15)0.0362 (7)
H3120.59990.07120.36070.043*
C4010.4056 (3)0.4445 (3)0.13947 (14)0.0298 (6)
C4020.3124 (3)0.5476 (3)0.13833 (16)0.0397 (8)
H4020.23960.55490.16050.048*
C4030.3264 (4)0.6402 (3)0.10452 (19)0.0488 (9)
H4030.26320.71010.10400.059*
C4040.4319 (4)0.6305 (3)0.07180 (18)0.0481 (9)
H4040.44090.69360.04910.058*
C4050.5241 (4)0.5287 (3)0.07225 (18)0.0478 (9)
H4050.59610.52210.04960.057*
C4060.5115 (3)0.4355 (3)0.10599 (16)0.0394 (8)
H4060.57520.36600.10620.047*
C4070.5050 (3)0.2106 (3)0.15751 (15)0.0316 (7)
C4080.4890 (4)0.1989 (3)0.09900 (18)0.0458 (9)
H4080.41770.25000.07350.055*
C4090.5773 (4)0.1125 (4)0.0779 (2)0.0590 (11)
H4090.56630.10510.03810.071*
C4100.6809 (5)0.0375 (4)0.1154 (2)0.0652 (13)
H4100.73950.02250.10160.078*
C4110.6996 (4)0.0494 (4)0.1723 (2)0.0665 (13)
H4110.77180.00170.19720.080*
C4120.6133 (4)0.1358 (3)0.19386 (18)0.0474 (9)
H4120.62760.14430.23290.057*
Cl10.26323 (9)0.19319 (10)0.33214 (5)0.0573 (3)
Cl20.17302 (11)0.07900 (9)0.26051 (5)0.0607 (3)
C130.3341 (7)0.8877 (5)0.1243 (3)0.097 (2)
H13A0.29760.92960.15550.117*
H13B0.35250.81080.14350.117*
Cl30.4728 (3)0.8992 (2)0.10094 (13)0.1458 (8)
Cl40.2257 (2)0.93632 (14)0.06158 (9)0.1169 (6)
C140.7130 (7)0.6657 (5)0.3733 (3)0.0917 (19)0.65
H14A0.76220.74370.35430.110*0.65
H14B0.74380.62360.35460.110*0.65
Cl50.7328 (5)0.6391 (3)0.45165 (15)0.1329 (15)0.65
Cl60.5546 (6)0.6307 (7)0.3585 (4)0.167 (3)0.65
C14A0.7130 (7)0.6657 (5)0.3733 (3)0.0917 (19)0.35
H14C0.71440.61990.34650.110*0.35
H14D0.74210.74060.34710.110*0.35
Cl5A0.832 (3)0.6662 (17)0.4298 (7)0.355 (14)0.35
Cl6A0.5736 (14)0.6287 (15)0.3920 (10)0.276 (12)0.35
O60.0892 (5)0.0527 (5)0.3189 (3)0.1181 (17)
H6OA0.013 (3)0.063 (6)0.316 (4)0.13 (3)*
H6OB0.133 (5)0.012 (2)0.323 (3)0.078 (19)*
O71.0377 (12)0.7546 (9)0.4039 (6)0.141 (4)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.02408 (6)0.02543 (7)0.02014 (6)0.01177 (5)0.00110 (4)0.00062 (4)
P10.0247 (4)0.0330 (4)0.0248 (4)0.0140 (3)0.0033 (3)0.0001 (3)
P20.0283 (4)0.0362 (4)0.0228 (4)0.0159 (3)0.0004 (3)0.0008 (3)
P30.0255 (4)0.0285 (4)0.0210 (3)0.0125 (3)0.0025 (3)0.0003 (3)
P40.0235 (4)0.0255 (4)0.0236 (4)0.0111 (3)0.0011 (3)0.0013 (3)
O10.0451 (14)0.0380 (13)0.0475 (14)0.0129 (11)0.0168 (12)0.0114 (11)
O20.0393 (13)0.0257 (11)0.0495 (14)0.0082 (10)0.0123 (11)0.0071 (10)
O30.0543 (17)0.077 (2)0.0410 (14)0.0398 (16)0.0130 (13)0.0048 (13)
O40.0694 (19)0.0627 (17)0.0328 (13)0.0365 (15)0.0086 (12)0.0165 (12)
O50.0646 (19)0.0441 (15)0.0625 (18)0.0250 (14)0.0087 (14)0.0249 (14)
C10.0271 (15)0.0310 (15)0.0190 (13)0.0142 (13)0.0007 (11)0.0018 (11)
C20.0299 (16)0.0413 (18)0.0273 (15)0.0217 (14)0.0020 (12)0.0010 (13)
C30.0251 (15)0.0302 (15)0.0267 (15)0.0138 (12)0.0009 (12)0.0017 (12)
C40.0233 (15)0.0288 (15)0.0230 (14)0.0083 (12)0.0001 (11)0.0041 (12)
C50.0318 (17)0.0286 (16)0.0303 (16)0.0083 (13)0.0024 (13)0.0066 (13)
C60.060 (3)0.0301 (18)0.067 (3)0.0143 (18)0.015 (2)0.0126 (18)
C70.098 (4)0.032 (2)0.134 (5)0.011 (2)0.055 (4)0.008 (3)
C80.0356 (17)0.0345 (17)0.0230 (15)0.0131 (14)0.0050 (13)0.0037 (12)
C90.0389 (19)0.0400 (18)0.0230 (15)0.0151 (15)0.0038 (13)0.0052 (13)
C100.086 (4)0.071 (3)0.039 (2)0.024 (3)0.003 (2)0.022 (2)
C110.161 (7)0.079 (4)0.070 (4)0.053 (4)0.006 (4)0.034 (3)
C120.0338 (17)0.0349 (17)0.0302 (16)0.0163 (14)0.0016 (13)0.0033 (14)
C1010.0306 (16)0.0398 (18)0.0325 (16)0.0190 (14)0.0019 (13)0.0043 (14)
C1020.062 (3)0.045 (2)0.052 (2)0.026 (2)0.0127 (19)0.0044 (18)
C1030.085 (3)0.051 (3)0.075 (3)0.038 (2)0.009 (3)0.018 (2)
C1040.070 (3)0.069 (3)0.056 (3)0.035 (2)0.013 (2)0.022 (2)
C1050.051 (2)0.065 (3)0.041 (2)0.028 (2)0.0091 (17)0.0112 (18)
C1060.042 (2)0.045 (2)0.0369 (18)0.0198 (17)0.0063 (15)0.0058 (15)
C1070.0288 (16)0.0409 (18)0.0290 (16)0.0123 (14)0.0037 (13)0.0045 (13)
C1080.0335 (18)0.0423 (19)0.0357 (18)0.0115 (15)0.0036 (14)0.0031 (15)
C1090.048 (2)0.044 (2)0.059 (2)0.0092 (18)0.0060 (19)0.0071 (19)
C1100.038 (2)0.062 (3)0.070 (3)0.000 (2)0.002 (2)0.018 (2)
C1110.032 (2)0.070 (3)0.068 (3)0.017 (2)0.0058 (19)0.016 (2)
C1120.0328 (18)0.055 (2)0.047 (2)0.0175 (17)0.0020 (15)0.0099 (17)
C2010.0348 (17)0.0460 (19)0.0253 (15)0.0225 (15)0.0028 (13)0.0055 (14)
C2020.063 (3)0.045 (2)0.0362 (19)0.0252 (19)0.0037 (17)0.0026 (16)
C2030.103 (4)0.043 (2)0.056 (3)0.030 (3)0.008 (3)0.010 (2)
C2040.096 (4)0.068 (3)0.046 (3)0.038 (3)0.009 (2)0.024 (2)
C2050.093 (4)0.084 (4)0.026 (2)0.042 (3)0.002 (2)0.008 (2)
C2060.068 (3)0.060 (3)0.0281 (18)0.028 (2)0.0005 (17)0.0002 (17)
C2070.0394 (19)0.047 (2)0.0286 (16)0.0144 (16)0.0083 (14)0.0062 (15)
C2080.068 (3)0.058 (3)0.041 (2)0.029 (2)0.0203 (19)0.0191 (19)
C2090.114 (5)0.075 (4)0.065 (3)0.035 (3)0.033 (3)0.041 (3)
C2100.090 (5)0.094 (5)0.096 (5)0.004 (4)0.031 (4)0.055 (4)
C2110.050 (3)0.133 (6)0.085 (4)0.001 (3)0.020 (3)0.049 (4)
C2120.040 (2)0.087 (3)0.048 (2)0.016 (2)0.0090 (18)0.021 (2)
C3010.0282 (16)0.0372 (17)0.0246 (15)0.0097 (13)0.0045 (12)0.0037 (13)
C3020.052 (2)0.051 (2)0.0295 (17)0.0227 (18)0.0041 (15)0.0013 (16)
C3030.080 (3)0.070 (3)0.0256 (18)0.028 (3)0.0077 (19)0.0006 (18)
C3040.070 (3)0.077 (3)0.030 (2)0.015 (2)0.0125 (19)0.016 (2)
C3050.068 (3)0.059 (3)0.048 (2)0.020 (2)0.019 (2)0.018 (2)
C3060.050 (2)0.043 (2)0.0374 (19)0.0162 (17)0.0116 (16)0.0079 (16)
C3070.0285 (16)0.0286 (15)0.0273 (15)0.0121 (13)0.0013 (12)0.0001 (12)
C3080.0355 (18)0.0368 (18)0.0402 (18)0.0157 (15)0.0040 (14)0.0036 (15)
C3090.058 (2)0.040 (2)0.056 (2)0.0215 (19)0.0046 (19)0.0138 (18)
C3100.055 (2)0.0330 (19)0.058 (2)0.0088 (18)0.0016 (19)0.0101 (17)
C3110.0363 (19)0.0384 (19)0.047 (2)0.0077 (16)0.0011 (16)0.0004 (16)
C3120.0350 (18)0.0348 (17)0.0353 (17)0.0149 (14)0.0019 (14)0.0014 (14)
C4010.0338 (16)0.0315 (16)0.0240 (14)0.0170 (13)0.0024 (12)0.0003 (12)
C4020.043 (2)0.0355 (18)0.0407 (19)0.0199 (16)0.0069 (15)0.0046 (15)
C4030.056 (2)0.0312 (18)0.055 (2)0.0185 (17)0.0004 (19)0.0017 (16)
C4040.061 (2)0.045 (2)0.043 (2)0.035 (2)0.0030 (18)0.0031 (16)
C4050.050 (2)0.054 (2)0.045 (2)0.0336 (19)0.0110 (17)0.0024 (17)
C4060.0371 (18)0.0406 (19)0.0423 (19)0.0222 (16)0.0083 (15)0.0041 (15)
C4070.0310 (16)0.0291 (16)0.0339 (16)0.0144 (13)0.0082 (13)0.0047 (13)
C4080.040 (2)0.051 (2)0.048 (2)0.0175 (17)0.0072 (16)0.0195 (18)
C4090.065 (3)0.064 (3)0.062 (3)0.032 (2)0.021 (2)0.035 (2)
C4100.063 (3)0.044 (2)0.075 (3)0.007 (2)0.021 (2)0.025 (2)
C4110.054 (3)0.048 (2)0.064 (3)0.004 (2)0.011 (2)0.006 (2)
C4120.038 (2)0.045 (2)0.041 (2)0.0052 (16)0.0055 (16)0.0030 (16)
Cl10.0438 (5)0.0810 (7)0.0495 (5)0.0391 (5)0.0037 (4)0.0043 (5)
Cl20.0611 (6)0.0621 (6)0.0573 (6)0.0275 (5)0.0059 (5)0.0071 (5)
C130.154 (6)0.068 (3)0.083 (4)0.052 (4)0.001 (4)0.031 (3)
Cl30.153 (2)0.1225 (17)0.162 (2)0.0639 (16)0.0071 (17)0.0252 (15)
Cl40.1430 (17)0.0734 (10)0.1140 (14)0.0276 (10)0.0145 (12)0.0223 (9)
C140.123 (5)0.071 (4)0.082 (4)0.041 (4)0.031 (4)0.012 (3)
Cl50.222 (5)0.0797 (17)0.0748 (18)0.050 (2)0.002 (2)0.0040 (14)
Cl60.092 (3)0.148 (4)0.213 (6)0.023 (3)0.027 (3)0.016 (4)
C14A0.123 (5)0.071 (4)0.082 (4)0.041 (4)0.031 (4)0.012 (3)
Cl5A0.63 (4)0.40 (2)0.173 (13)0.38 (3)0.003 (18)0.010 (14)
Cl6A0.169 (13)0.207 (13)0.47 (3)0.030 (9)0.151 (16)0.171 (18)
O60.084 (4)0.102 (4)0.173 (5)0.049 (3)0.035 (4)0.031 (4)
O70.137 (10)0.108 (8)0.188 (12)0.055 (7)0.021 (9)0.049 (8)
Geometric parameters (Å, º) top
Ir1—C121.910 (3)C203—H2030.9400
Ir1—C42.119 (3)C204—C2051.361 (7)
Ir1—C82.177 (3)C204—H2040.9400
Ir1—C12.225 (3)C205—C2061.385 (6)
Ir1—P12.3393 (8)C205—H2050.9400
Ir1—P42.3658 (8)C206—H2060.9400
P1—C1011.811 (3)C207—C2081.382 (6)
P1—C1071.822 (3)C207—C2121.385 (6)
P1—C21.839 (3)C208—C2091.381 (6)
P2—C2011.800 (3)C208—H2080.9400
P2—C2071.802 (4)C209—C2101.353 (9)
P2—C21.810 (3)C209—H2090.9400
P2—C11.837 (3)C210—C2111.380 (10)
P3—C11.791 (3)C210—H2100.9400
P3—C31.798 (3)C211—C2121.398 (7)
P3—C3071.804 (3)C211—H2110.9400
P3—C3011.808 (3)C212—H2120.9400
P4—C4071.820 (3)C301—C3061.387 (5)
P4—C4011.821 (3)C301—C3021.390 (5)
P4—C31.840 (3)C302—C3031.381 (5)
O1—C51.208 (4)C302—H3020.9400
O2—C51.340 (4)C303—C3041.364 (7)
O2—C61.468 (4)C303—H3030.9400
O3—C91.205 (4)C304—C3051.374 (7)
O4—C91.348 (4)C304—H3040.9400
O4—C101.446 (5)C305—C3061.393 (5)
O5—C121.120 (4)C305—H3050.9400
C1—C41.515 (4)C306—H3060.9400
C2—H2A0.9800C307—C3081.392 (5)
C2—H2B0.9800C307—C3121.398 (4)
C3—H3A0.9800C308—C3091.388 (5)
C3—H3B0.9800C308—H3080.9400
C4—C51.488 (4)C309—C3101.376 (6)
C4—H40.942 (18)C309—H3090.9400
C6—C71.479 (6)C310—C3111.381 (6)
C6—H6A0.9800C310—H3100.9400
C6—H6B0.9800C311—C3121.384 (5)
C7—H7A0.9700C311—H3110.9400
C7—H7B0.9700C312—H3120.9400
C7—H7C0.9700C401—C4021.385 (5)
C8—C91.470 (5)C401—C4061.386 (5)
C8—H8A0.9800C402—C4031.386 (5)
C8—H8B0.9800C402—H4020.9400
C10—C111.485 (8)C403—C4041.371 (6)
C10—H10A0.9800C403—H4030.9400
C10—H10B0.9800C404—C4051.371 (6)
C11—H11A0.9700C404—H4040.9400
C11—H11B0.9700C405—C4061.385 (5)
C11—H11C0.9700C405—H4050.9400
C101—C1021.388 (5)C406—H4060.9400
C101—C1061.394 (5)C407—C4081.385 (5)
C102—C1031.389 (6)C407—C4121.395 (5)
C102—H1020.9400C408—C4091.383 (5)
C103—C1041.363 (6)C408—H4080.9400
C103—H1030.9400C409—C4101.373 (7)
C104—C1051.359 (6)C409—H4090.9400
C104—H1040.9400C410—C4111.359 (7)
C105—C1061.384 (5)C410—H4100.9400
C105—H1050.9400C411—C4121.380 (6)
C106—H1060.9400C411—H4110.9400
C107—C1081.389 (5)C412—H4120.9400
C107—C1121.398 (5)C13—Cl31.736 (8)
C108—C1091.383 (5)C13—Cl41.746 (7)
C108—H1080.9400C13—H13A0.9800
C109—C1101.386 (7)C13—H13B0.9800
C109—H1090.9400C14—Cl51.713 (7)
C110—C1111.385 (7)C14—Cl61.745 (10)
C110—H1100.9400C14—H14A0.9800
C111—C1121.370 (6)C14—H14B0.9800
C111—H1110.9400C14A—Cl6A1.545 (15)
C112—H1120.9400C14A—Cl5A1.82 (2)
C201—C2021.381 (5)C14A—H14C0.9800
C201—C2061.403 (5)C14A—H14D0.9800
C202—C2031.380 (5)O6—H6OA0.85 (2)
C202—H2020.9400O6—H6OB0.845 (19)
C203—C2041.377 (7)
C12—Ir1—C4158.78 (12)C112—C111—H111119.9
C12—Ir1—C893.36 (13)C110—C111—H111119.9
C4—Ir1—C8106.70 (12)C111—C112—C107120.2 (4)
C12—Ir1—C1118.82 (12)C111—C112—H112119.9
C4—Ir1—C140.72 (11)C107—C112—H112119.9
C8—Ir1—C1147.39 (12)C202—C201—C206119.1 (3)
C12—Ir1—P188.65 (10)C202—C201—P2121.8 (3)
C4—Ir1—P185.11 (9)C206—C201—P2118.9 (3)
C8—Ir1—P188.50 (9)C203—C202—C201120.2 (4)
C1—Ir1—P187.22 (8)C203—C202—H202119.9
C12—Ir1—P491.76 (10)C201—C202—H202119.9
C4—Ir1—P493.24 (8)C204—C203—C202120.5 (5)
C8—Ir1—P495.09 (9)C204—C203—H203119.7
C1—Ir1—P489.41 (8)C202—C203—H203119.7
P1—Ir1—P4176.35 (3)C205—C204—C203119.9 (4)
C101—P1—C107102.78 (15)C205—C204—H204120.1
C101—P1—C2106.38 (15)C203—C204—H204120.1
C107—P1—C2105.77 (15)C204—C205—C206120.9 (4)
C101—P1—Ir1116.72 (11)C204—C205—H205119.6
C107—P1—Ir1120.29 (11)C206—C205—H205119.6
C2—P1—Ir1103.76 (10)C205—C206—C201119.4 (4)
C201—P2—C207105.53 (16)C205—C206—H206120.3
C201—P2—C2107.18 (15)C201—C206—H206120.3
C207—P2—C2110.99 (17)C208—C207—C212120.6 (4)
C201—P2—C1120.40 (15)C208—C207—P2119.7 (3)
C207—P2—C1107.20 (16)C212—C207—P2119.7 (3)
C2—P2—C1105.50 (14)C209—C208—C207120.2 (5)
C1—P3—C3106.12 (14)C209—C208—H208119.9
C1—P3—C307111.84 (14)C207—C208—H208119.9
C3—P3—C307107.34 (14)C210—C209—C208120.1 (6)
C1—P3—C301117.32 (14)C210—C209—H209120.0
C3—P3—C301108.18 (15)C208—C209—H209120.0
C307—P3—C301105.63 (15)C209—C210—C211120.3 (5)
C407—P4—C401104.51 (14)C209—C210—H210119.9
C407—P4—C3105.94 (15)C211—C210—H210119.9
C401—P4—C3103.41 (14)C210—C211—C212121.1 (5)
C407—P4—Ir1116.18 (11)C210—C211—H211119.5
C401—P4—Ir1119.97 (11)C212—C211—H211119.5
C3—P4—Ir1105.34 (10)C207—C212—C211117.7 (5)
C5—O2—C6116.8 (3)C207—C212—H212121.1
C9—O4—C10116.1 (3)C211—C212—H212121.1
C4—C1—P3121.7 (2)C306—C301—C302119.5 (3)
C4—C1—P2108.3 (2)C306—C301—P3122.3 (3)
P3—C1—P2122.16 (16)C302—C301—P3118.2 (3)
C4—C1—Ir165.88 (15)C303—C302—C301119.8 (4)
P3—C1—Ir1110.27 (14)C303—C302—H302120.1
P2—C1—Ir1115.59 (14)C301—C302—H302120.1
P2—C2—P1111.79 (17)C304—C303—C302120.5 (4)
P2—C2—H2A109.3C304—C303—H303119.8
P1—C2—H2A109.3C302—C303—H303119.8
P2—C2—H2B109.3C303—C304—C305120.7 (4)
P1—C2—H2B109.3C303—C304—H304119.6
H2A—C2—H2B107.9C305—C304—H304119.6
P3—C3—P4110.67 (16)C304—C305—C306119.6 (4)
P3—C3—H3A109.5C304—C305—H305120.2
P4—C3—H3A109.5C306—C305—H305120.2
P3—C3—H3B109.5C301—C306—C305119.9 (4)
P4—C3—H3B109.5C301—C306—H306120.1
H3A—C3—H3B108.1C305—C306—H306120.1
C5—C4—C1125.7 (3)C308—C307—C312119.2 (3)
C5—C4—Ir1131.9 (2)C308—C307—P3124.0 (2)
C1—C4—Ir173.40 (16)C312—C307—P3116.5 (2)
C5—C4—H4104 (2)C309—C308—C307119.9 (3)
C1—C4—H4112 (2)C309—C308—H308120.1
Ir1—C4—H4108 (2)C307—C308—H308120.1
O1—C5—O2122.8 (3)C310—C309—C308120.4 (4)
O1—C5—C4127.9 (3)C310—C309—H309119.8
O2—C5—C4109.2 (3)C308—C309—H309119.8
O2—C6—C7106.6 (3)C309—C310—C311120.3 (4)
O2—C6—H6A110.4C309—C310—H310119.8
C7—C6—H6A110.4C311—C310—H310119.8
O2—C6—H6B110.4C310—C311—C312119.9 (3)
C7—C6—H6B110.4C310—C311—H311120.0
H6A—C6—H6B108.6C312—C311—H311120.0
C6—C7—H7A109.5C311—C312—C307120.2 (3)
C6—C7—H7B109.5C311—C312—H312119.9
H7A—C7—H7B109.5C307—C312—H312119.9
C6—C7—H7C109.5C402—C401—C406119.1 (3)
H7A—C7—H7C109.5C402—C401—P4119.2 (2)
H7B—C7—H7C109.5C406—C401—P4121.7 (3)
C9—C8—Ir1114.1 (2)C401—C402—C403120.0 (3)
C9—C8—H8A108.7C401—C402—H402120.0
Ir1—C8—H8A108.7C403—C402—H402120.0
C9—C8—H8B108.7C404—C403—C402120.4 (4)
Ir1—C8—H8B108.7C404—C403—H403119.8
H8A—C8—H8B107.6C402—C403—H403119.8
O3—C9—O4122.3 (3)C405—C404—C403120.0 (3)
O3—C9—C8126.2 (3)C405—C404—H404120.0
O4—C9—C8111.5 (3)C403—C404—H404120.0
O4—C10—C11107.2 (5)C404—C405—C406120.2 (4)
O4—C10—H10A110.3C404—C405—H405119.9
C11—C10—H10A110.3C406—C405—H405119.9
O4—C10—H10B110.3C405—C406—C401120.3 (3)
C11—C10—H10B110.3C405—C406—H406119.9
H10A—C10—H10B108.5C401—C406—H406119.9
C10—C11—H11A109.5C408—C407—C412118.9 (3)
C10—C11—H11B109.5C408—C407—P4118.6 (3)
H11A—C11—H11B109.5C412—C407—P4122.6 (3)
C10—C11—H11C109.5C409—C408—C407120.4 (4)
H11A—C11—H11C109.5C409—C408—H408119.8
H11B—C11—H11C109.5C407—C408—H408119.8
O5—C12—Ir1177.9 (3)C410—C409—C408119.7 (4)
C102—C101—C106119.1 (3)C410—C409—H409120.2
C102—C101—P1122.4 (3)C408—C409—H409120.2
C106—C101—P1118.2 (3)C411—C410—C409120.6 (4)
C101—C102—C103119.3 (4)C411—C410—H410119.7
C101—C102—H102120.4C409—C410—H410119.7
C103—C102—H102120.4C410—C411—C412120.5 (4)
C104—C103—C102120.7 (4)C410—C411—H411119.7
C104—C103—H103119.6C412—C411—H411119.7
C102—C103—H103119.6C411—C412—C407119.8 (4)
C105—C104—C103120.7 (4)C411—C412—H412120.1
C105—C104—H104119.7C407—C412—H412120.1
C103—C104—H104119.7Cl3—C13—Cl4111.3 (4)
C104—C105—C106120.0 (4)Cl3—C13—H13A109.4
C104—C105—H105120.0Cl4—C13—H13A109.4
C106—C105—H105120.0Cl3—C13—H13B109.4
C105—C106—C101120.2 (4)Cl4—C13—H13B109.4
C105—C106—H106119.9H13A—C13—H13B108.0
C101—C106—H106119.9Cl5—C14—Cl6110.5 (4)
C108—C107—C112119.1 (3)Cl5—C14—H14A109.6
C108—C107—P1123.4 (3)Cl6—C14—H14A109.6
C112—C107—P1117.5 (3)Cl5—C14—H14B109.6
C109—C108—C107120.7 (4)Cl6—C14—H14B109.6
C109—C108—H108119.7H14A—C14—H14B108.1
C107—C108—H108119.7Cl6A—C14A—Cl5A123.0 (11)
C108—C109—C110119.4 (4)Cl6A—C14A—H14C106.6
C108—C109—H109120.3Cl5A—C14A—H14C106.6
C110—C109—H109120.3Cl6A—C14A—H14D106.6
C111—C110—C109120.3 (4)Cl5A—C14A—H14D106.6
C111—C110—H110119.9H14C—C14A—H14D106.5
C109—C110—H110119.9H6OA—O6—H6OB109 (7)
C112—C111—C110120.3 (4)
C3—P3—C1—C432.3 (3)C1—P2—C201—C206101.9 (3)
C307—P3—C1—C4149.1 (2)C206—C201—C202—C2031.9 (6)
C301—P3—C1—C488.7 (3)P2—C201—C202—C203176.6 (4)
C3—P3—C1—P2177.92 (18)C201—C202—C203—C2041.0 (8)
C307—P3—C1—P265.3 (2)C202—C203—C204—C2050.1 (9)
C301—P3—C1—P256.9 (2)C203—C204—C205—C2060.4 (9)
C3—P3—C1—Ir141.19 (18)C204—C205—C206—C2010.5 (8)
C307—P3—C1—Ir175.56 (17)C202—C201—C206—C2051.6 (6)
C301—P3—C1—Ir1162.17 (14)P2—C201—C206—C205176.5 (4)
C201—P2—C1—C4159.6 (2)C201—P2—C207—C20891.7 (3)
C207—P2—C1—C439.2 (2)C2—P2—C207—C208152.5 (3)
C2—P2—C1—C479.2 (2)C1—P2—C207—C20837.7 (3)
C201—P2—C1—P310.0 (3)C201—P2—C207—C21286.1 (3)
C207—P2—C1—P3110.4 (2)C2—P2—C207—C21229.7 (4)
C2—P2—C1—P3131.2 (2)C1—P2—C207—C212144.4 (3)
C201—P2—C1—Ir1128.96 (17)C212—C207—C208—C2091.7 (6)
C207—P2—C1—Ir1110.60 (17)P2—C207—C208—C209179.5 (4)
C2—P2—C1—Ir17.8 (2)C207—C208—C209—C2100.1 (8)
C201—P2—C2—P1163.12 (18)C208—C209—C210—C2111.4 (10)
C207—P2—C2—P182.1 (2)C209—C210—C211—C2121.4 (11)
C1—P2—C2—P133.7 (2)C208—C207—C212—C2111.6 (6)
C101—P1—C2—P2167.17 (18)P2—C207—C212—C211179.4 (4)
C107—P1—C2—P284.0 (2)C210—C211—C212—C2070.1 (9)
Ir1—P1—C2—P243.49 (19)C1—P3—C301—C30696.7 (3)
C1—P3—C3—P445.4 (2)C3—P3—C301—C30623.2 (3)
C307—P3—C3—P474.32 (19)C307—P3—C301—C306137.9 (3)
C301—P3—C3—P4172.12 (15)C1—P3—C301—C30285.3 (3)
C407—P4—C3—P394.87 (18)C3—P3—C301—C302154.8 (3)
C401—P4—C3—P3155.50 (17)C307—P3—C301—C30240.1 (3)
Ir1—P4—C3—P328.78 (17)C306—C301—C302—C3031.6 (6)
P3—C1—C4—C530.3 (4)P3—C301—C302—C303179.7 (3)
P2—C1—C4—C5119.4 (3)C301—C302—C303—C3041.3 (7)
Ir1—C1—C4—C5130.1 (3)C302—C303—C304—C3050.2 (8)
P3—C1—C4—Ir199.8 (2)C303—C304—C305—C3060.4 (7)
P2—C1—C4—Ir1110.49 (16)C302—C301—C306—C3051.0 (6)
C6—O2—C5—O10.8 (5)P3—C301—C306—C305179.0 (3)
C6—O2—C5—C4177.3 (3)C304—C305—C306—C3010.0 (6)
C1—C4—C5—O12.1 (5)C1—P3—C307—C30810.8 (3)
Ir1—C4—C5—O197.9 (4)C3—P3—C307—C308105.2 (3)
C1—C4—C5—O2175.9 (3)C301—P3—C307—C308139.5 (3)
Ir1—C4—C5—O284.2 (3)C1—P3—C307—C312174.7 (2)
C5—O2—C6—C7171.6 (4)C3—P3—C307—C31269.3 (3)
C10—O4—C9—O32.9 (5)C301—P3—C307—C31246.0 (3)
C10—O4—C9—C8175.7 (3)C312—C307—C308—C3090.6 (5)
Ir1—C8—C9—O395.1 (4)P3—C307—C308—C309175.0 (3)
Ir1—C8—C9—O483.4 (3)C307—C308—C309—C3101.7 (6)
C9—O4—C10—C11178.5 (4)C308—C309—C310—C3111.1 (6)
C107—P1—C101—C102143.3 (3)C309—C310—C311—C3120.5 (6)
C2—P1—C101—C10232.4 (4)C310—C311—C312—C3071.6 (5)
Ir1—P1—C101—C10282.8 (3)C308—C307—C312—C3111.0 (5)
C107—P1—C101—C10642.1 (3)P3—C307—C312—C311173.8 (3)
C2—P1—C101—C106153.0 (3)C407—P4—C401—C402166.4 (3)
Ir1—P1—C101—C10691.8 (3)C3—P4—C401—C40282.9 (3)
C106—C101—C102—C1031.9 (6)Ir1—P4—C401—C40234.0 (3)
P1—C101—C102—C103176.5 (4)C407—P4—C401—C40612.3 (3)
C101—C102—C103—C1041.2 (7)C3—P4—C401—C40698.4 (3)
C102—C103—C104—C1050.1 (8)Ir1—P4—C401—C406144.8 (2)
C103—C104—C105—C1060.1 (7)C406—C401—C402—C4030.6 (5)
C104—C105—C106—C1010.6 (6)P4—C401—C402—C403179.4 (3)
C102—C101—C106—C1051.6 (6)C401—C402—C403—C4040.3 (6)
P1—C101—C106—C105176.4 (3)C402—C403—C404—C4050.2 (6)
C101—P1—C107—C108121.0 (3)C403—C404—C405—C4060.4 (6)
C2—P1—C107—C108127.6 (3)C404—C405—C406—C4010.1 (6)
Ir1—P1—C107—C10810.8 (3)C402—C401—C406—C4050.4 (5)
C101—P1—C107—C11257.8 (3)P4—C401—C406—C405179.1 (3)
C2—P1—C107—C11253.6 (3)C401—P4—C407—C40873.7 (3)
Ir1—P1—C107—C112170.4 (2)C3—P4—C407—C408177.4 (3)
C112—C107—C108—C1091.7 (5)Ir1—P4—C407—C40860.9 (3)
P1—C107—C108—C109179.5 (3)C401—P4—C407—C412105.6 (3)
C107—C108—C109—C1100.5 (6)C3—P4—C407—C4123.3 (3)
C108—C109—C110—C1110.6 (7)Ir1—P4—C407—C412119.8 (3)
C109—C110—C111—C1120.5 (7)C412—C407—C408—C4092.0 (6)
C110—C111—C112—C1070.8 (6)P4—C407—C408—C409178.7 (3)
C108—C107—C112—C1111.8 (5)C407—C408—C409—C4100.4 (7)
P1—C107—C112—C111179.3 (3)C408—C409—C410—C4112.1 (7)
C207—P2—C201—C202155.4 (3)C409—C410—C411—C4121.3 (8)
C2—P2—C201—C20237.0 (3)C410—C411—C412—C4071.2 (7)
C1—P2—C201—C20283.3 (3)C408—C407—C412—C4112.8 (6)
C207—P2—C201—C20619.4 (3)P4—C407—C412—C411177.9 (3)
C2—P2—C201—C206137.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2A···Cl10.982.483.421 (3)162
C3—H3A···Cl1i0.982.593.488 (3)152
C3—H3B···O10.982.212.968 (4)134
C102—H102···Cl20.942.613.505 (4)160
C108—H108···O20.942.613.313 (4)132
C112—H112···Cl10.942.803.595 (4)143
C202—H202···Cl20.942.703.574 (4)156
C212—H212···Cl10.942.803.733 (5)173
C306—H306···O10.942.473.061 (4)121
C312—H312···Cl1i0.942.733.503 (4)140
C402—H402···O20.942.473.375 (4)162
C408—H408···O30.942.443.326 (5)156
C412—H412···Cl1i0.942.973.866 (4)161
C13—H13A···O5ii0.982.583.194 (6)121
C13—H13A···Cl2ii0.982.683.500 (7)141
C14—H14A···Cl2iii0.982.653.553 (6)153
C14—H14B···O1iv0.982.373.327 (6)164
C14A—H14C···O1iv0.982.383.327 (6)163
C14A—H14D···Cl2iii0.982.593.553 (6)168
O6—H6OA···Cl20.85 (2)2.39 (4)3.178 (5)154 (7)
O6—H6OB···Cl10.85 (2)2.39 (2)3.239 (6)178 (6)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z; (iii) x1, y+1, z; (iv) x1, y, z.
Selected bond lengths (Å) and angles (°) of the compounds 4, 5, 6 and 7 top
4567
Ir1—C12.273 (4)2.279 (6)2.149 (4)2.225 (3)
Ir1—C42.072 (5)2.046 (7)2.076 (4)2.119 (3)
Ir1—P12.290 (1)2.318 (2)2.309 (1)2.339 (1)
Ir1—P42.278 (1)2.306 (2)2.330 (1)2.366 (1)
P2—C11.791 (5)1.788 (7)1.822 (4)1.837 (3)
Ir1—Lx (Lx= –H, –Cl, –CH2CO2Et)1.62 (2)2.163 (7)2.427 (1)2.177 (3)
Ir1—Ly (Ly = –Cl, –CO)2.462 (1)2.461 (2)2.460 (1)1.910 (3)
P3—C11.788 (5)1.789 (7)1.833 (4)1.791 (3)
C1—C41.515 (6)1.507 (9)1.513 (5)1.515 (4)
C4—Ir1—C140.5 (2)40.3 (2)41.9 (2)40.72 (11)
C4—C1—Ir162.6 (2)61.5 (3)66.5 (2)65.88 (15)
C1—C4—Ir176.9 (3)78.2 (4)71.6 (2)73.40 (16)
C4—Ir1—Ly (Ly = –Cl, –CO)150.3 (1)152.5 (2)151.9 (1)158.8 (1)
C1—Ir1—Ly (Ly = –Cl, –CO)111.3 (1)112.8 (2)111.5 (1)118.8 (1)
C4—Ir1—Lx (Lx= –H, –Cl, –CH2CO2Et)119.7 (18)120.8 (3)116.2 (1)106.7 (1)
C1—Ir1—Lx (Lx=-H, -Cl, -CH2CO2Et)159.8 (18)161.1 (3)158.1 (1)147.4 (1)
P1—Ir1—P4178.4 (1)173.5 (1)177.6 (1)176.4 (1)
P1—Ir1—(C1-C4)84.2188.8585.5784.56
 

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