Chiral MOP-phosphonite ligands: synthesis, characterisation and interconversion of η(1),η(6)-(σ-P, π-arene) chelated rhodium(i) complexes.
Ficks, Arne; Harrington, Ross W.; Higham, Lee J.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 6302–6305; doi:10.1039/c3dt50482d

data_7021309
_publ_section_title
;
 Chiral MOP-phosphonite ligands: synthesis, characterisation and
 interconversion of \h(1),\h(6)-(\s-P, \p-arene) chelated rhodium(i)
 complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6302
_journal_page_last               6305
_journal_paper_doi               10.1039/c3dt50482d
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C49 H39 Cl Ir O3 P, C H2 Cl2'
_chemical_formula_sum            'C50 H41 Cl3 Ir O3 P'
_chemical_formula_weight         1019.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3945(2)
_cell_length_b                   19.2373(5)
_cell_length_c                   23.8082(5)
_cell_measurement_reflns_used    15162
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5717
_cell_measurement_theta_min      2.9522
_cell_volume                     4302.73(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24836
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    3.369
_exptl_absorpt_correction_T_max  0.5522
_exptl_absorpt_correction_T_min  0.4314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Fri Nov 11 12:12:35 2011'
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+2.3943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                8788
_reflns_number_total             9076
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50482d.txt
_cod_data_source_block           ljh149_2a
_cod_database_code               7021309
_computing_special_details
;
TITL ljh149 in P2(1)2(1)2(1)
CELL 0.71073 9.3945 19.2373 23.8082 90.000 90.000 90.000
ZERR 4.00 0.0002 0.0005 0.0005 0.000 0.000 0.000
LATT -1
SYMM 0.50000-X,-Y, 0.50000+Z
SYMM 0.50000+X, 0.50000-Y,-Z
SYMM -X, 0.50000+Y, 0.50000-Z
SFAC C H O P CL IR
UNIT 200 164 12 4 12 4
TEMP -123
ACTA 50
L.S. 8
LIST 1
FMAP 2
PLAN 10
OMIT 0 3 1
OMIT 0 1 4
OMIT 0 0 6
BOND $H
CONF
SIZE 0.30 0.20 0.20
REM red block
REM one DCM squeezed
REM EXTI 0.000208
WGHT 0.030100 2.394300
FVAR 2.04239
IR 6 0.767124 0.955114 0.707068 11.00000 0.01964 0.02537 =
0.01483 -0.00418 -0.00048 -0.00501
P 4 0.765100 0.986567 0.617172 11.00000 0.01633 0.01984 =
0.01686 -0.00342 0.00117 -0.00191
CL 5 0.567680 0.886842 0.683647 11.00000 0.02488 0.03038 =
0.01968 0.00100 -0.00289 -0.01039
O1 3 0.879715 1.046215 0.601239 11.00000 0.02074 0.02059 =
0.02352 -0.00151 0.00289 -0.00200
O2 3 0.616162 1.024032 0.600189 11.00000 0.01748 0.02269 =
0.02077 -0.00257 0.00127 0.00054
O3 3 1.126338 0.939675 0.576195 11.00000 0.01939 0.05687 =
0.05191 -0.02115 -0.00337 -0.00533
C1 1 0.857265 1.085583 0.552360 11.00000 0.02166 0.01752 =
0.02248 -0.00299 0.00509 -0.00529
C2 1 0.944746 1.071149 0.506220 11.00000 0.02692 0.02204 =
0.03087 -0.00389 0.01207 0.00086
AFIX 43
H2A 2 1.013982 1.035235 0.508148 11.00000 -1.20000
AFIX 0
C3 1 0.929039 1.109239 0.458780 11.00000 0.03216 0.02650 =
0.02939 -0.00359 0.01661 -0.00481
AFIX 43
H3A 2 0.990906 1.101301 0.427875 11.00000 -1.20000
AFIX 0
C4 1 0.821491 1.160870 0.454522 11.00000 0.03315 0.02277 =
0.02417 -0.00393 0.01046 -0.00393
C5 1 0.801149 1.199901 0.404486 11.00000 0.04325 0.03521 =
0.02331 0.00068 0.00786 -0.00711
AFIX 43
H5A 2 0.862910 1.192451 0.373469 11.00000 -1.20000
AFIX 0
C6 1 0.696234 1.247176 0.400143 11.00000 0.05032 0.03950 =
0.02536 0.00524 0.00058 -0.00253
AFIX 43
H6A 2 0.685295 1.273240 0.366527 11.00000 -1.20000
AFIX 0
C7 1 0.602500 1.257983 0.445581 11.00000 0.04490 0.03105 =
0.02931 0.00053 -0.00527 0.00569
AFIX 43
H7A 2 0.527319 1.290728 0.442106 11.00000 -1.20000
AFIX 0
C8 1 0.618829 1.221677 0.494738 11.00000 0.03227 0.03305 =
0.02229 -0.00435 0.00387 0.00444
AFIX 43
H8A 2 0.554557 1.229519 0.524885 11.00000 -1.20000
AFIX 0
C9 1 0.729029 1.173146 0.501144 11.00000 0.02691 0.02278 =
0.02175 -0.00426 0.00565 -0.00236
C10 1 0.752975 1.135524 0.552145 11.00000 0.02426 0.01868 =
0.01865 -0.00254 0.00418 -0.00106
C11 1 0.663711 1.145645 0.603498 11.00000 0.01965 0.02331 =
0.01960 -0.00518 0.00139 0.00328
C12 1 0.651439 1.210785 0.631275 11.00000 0.02349 0.02844 =
0.01959 -0.00601 -0.00326 0.00901
C13 1 0.725496 1.270871 0.615067 11.00000 0.02634 0.02962 =
0.02438 -0.00334 -0.00214 0.00386
AFIX 43
H13A 2 0.787660 1.268813 0.583639 11.00000 -1.20000
AFIX 0
C14 1 0.710549 1.332125 0.643253 11.00000 0.03340 0.02559 =
0.03419 -0.00781 -0.01323 0.00512
AFIX 43
H14A 2 0.759850 1.372449 0.630917 11.00000 -1.20000
AFIX 0
C15 1 0.621325 1.335228 0.690889 11.00000 0.03436 0.03053 =
0.02890 -0.01581 -0.01564 0.01414
AFIX 43
H15A 2 0.611002 1.377792 0.710709 11.00000 -1.20000
AFIX 0
C16 1 0.550770 1.278355 0.708446 11.00000 0.02725 0.04391 =
0.02338 -0.01650 -0.00823 0.01466
AFIX 43
H16A 2 0.491370 1.281462 0.740641 11.00000 -1.20000
AFIX 0
C17 1 0.562967 1.214583 0.680273 11.00000 0.02438 0.03343 =
0.01758 -0.00642 -0.00459 0.00946
C18 1 0.492049 1.154083 0.699522 11.00000 0.02309 0.04519 =
0.02022 -0.00381 0.00418 0.00886
AFIX 43
H18A 2 0.431160 1.157052 0.731289 11.00000 -1.20000
AFIX 0
C19 1 0.509476 1.092351 0.673532 11.00000 0.01925 0.03841 =
0.01983 -0.00157 0.00380 0.00024
AFIX 43
H19A 2 0.463548 1.051814 0.687349 11.00000 -1.20000
AFIX 0
C20 1 0.596778 1.089050 0.625651 11.00000 0.01719 0.02801 =
0.01563 -0.00779 0.00153 0.00246
C21 1 0.775324 0.926573 0.558297 11.00000 0.01769 0.01714 =
0.01600 -0.00204 0.00336 -0.00265
C22 1 0.689228 0.939101 0.510783 11.00000 0.02717 0.01883 =
0.01930 0.00204 0.00039 0.00324
AFIX 43
H22A 2 0.622653 0.976270 0.511109 11.00000 -1.20000
AFIX 0
C23 1 0.701502 0.897809 0.464273 11.00000 0.02807 0.02525 =
0.01600 0.00145 -0.00434 0.00186
AFIX 43
H23A 2 0.642662 0.906491 0.432589 11.00000 -1.20000
AFIX 0
C24 1 0.799244 0.843013 0.462586 11.00000 0.01856 0.02376 =
0.01776 -0.00168 0.00004 -0.00315
C25 1 0.814569 0.800072 0.413988 11.00000 0.02918 0.03087 =
0.01520 -0.00170 -0.00174 0.00130
AFIX 43
H25A 2 0.756402 0.808122 0.382002 11.00000 -1.20000
AFIX 0
C26 1 0.911752 0.747833 0.413240 11.00000 0.03316 0.03222 =
0.02024 -0.00736 0.00188 0.00037
AFIX 43
H26A 2 0.922692 0.720462 0.380310 11.00000 -1.20000
AFIX 0
C27 1 0.995833 0.733841 0.460283 11.00000 0.02921 0.03362 =
0.03145 -0.01015 -0.00048 0.01196
AFIX 43
H27A 2 1.061685 0.696382 0.459360 11.00000 -1.20000
AFIX 0
C28 1 0.984140 0.773610 0.507641 11.00000 0.02558 0.03683 =
0.02217 -0.00518 -0.00327 0.00694
AFIX 43
H28A 2 1.042935 0.763807 0.539125 11.00000 -1.20000
AFIX 0
C29 1 0.885821 0.829098 0.510423 11.00000 0.01698 0.02470 =
0.01968 -0.00170 0.00145 0.00064
C30 1 0.872124 0.872588 0.559003 11.00000 0.01289 0.02909 =
0.01609 -0.00228 -0.00078 0.00050
C31 1 0.965792 0.856528 0.608607 11.00000 0.02032 0.04156 =
0.02033 -0.01467 -0.00397 0.01103
C32 1 0.928249 0.801088 0.645177 11.00000 0.03398 0.04387 =
0.01567 -0.00689 -0.00608 0.02333
C33 1 0.801091 0.762715 0.640452 11.00000 0.03884 0.04245 =
0.02134 0.00274 0.00169 0.01277
AFIX 43
H33A 2 0.736290 0.774073 0.611227 11.00000 -1.20000
AFIX 0
C34 1 0.767705 0.710113 0.676106 11.00000 0.06544 0.04234 =
0.03313 0.00770 0.00596 0.01293
AFIX 43
H34A 2 0.680049 0.686037 0.671933 11.00000 -1.20000
AFIX 0
C35 1 0.862847 0.691057 0.719382 11.00000 0.08604 0.06045 =
0.03581 0.01441 0.00882 0.03481
AFIX 43
H35A 2 0.839569 0.654148 0.744249 11.00000 -1.20000
AFIX 0
C36 1 0.985005 0.725030 0.725104 11.00000 0.07838 0.07489 =
0.01938 0.00557 -0.00795 0.05125
AFIX 43
H36A 2 1.048394 0.711654 0.754254 11.00000 -1.20000
AFIX 0
C37 1 1.024352 0.781141 0.688805 11.00000 0.04497 0.06845 =
0.01873 -0.01138 -0.01193 0.03357
C38 1 1.151860 0.816116 0.693394 11.00000 0.05359 0.08908 =
0.02240 -0.02010 -0.01908 0.04303
AFIX 43
H38A 2 1.216751 0.802457 0.721938 11.00000 -1.20000
AFIX 0
C39 1 1.188772 0.869613 0.658588 11.00000 0.02144 0.08807 =
0.04436 -0.04437 -0.01627 0.01819
AFIX 43
H39A 2 1.276739 0.893192 0.663528 11.00000 -1.20000
AFIX 0
C40 1 1.093861 0.889676 0.614773 11.00000 0.02322 0.05168 =
0.03173 -0.01860 -0.00526 0.00896
C48 1 0.709631 0.949294 0.797850 11.00000 0.03715 0.04290 =
0.01358 -0.00097 0.00248 -0.01767
AFIX 13
H48A 2 0.609661 0.934216 0.805575 11.00000 -1.20000
AFIX 0
C45 1 0.861298 1.048349 0.734343 11.00000 0.03169 0.02734 =
0.02309 -0.00994 0.00035 -0.01063
AFIX 13
H45A 2 0.866788 1.084962 0.704606 11.00000 -1.20000
AFIX 0
C46 1 0.796510 1.073572 0.789168 11.00000 0.03765 0.03540 =
0.03105 -0.01850 0.00109 -0.00349
AFIX 23
H46A 2 0.709830 1.100896 0.780694 11.00000 -1.20000
H46B 2 0.865067 1.104894 0.808056 11.00000 -1.20000
AFIX 0
C43 1 1.036568 0.961557 0.780558 11.00000 0.02525 0.05964 =
0.02937 -0.01738 -0.00769 -0.00103
AFIX 23
H43A 2 1.043364 0.996060 0.811294 11.00000 -1.20000
H43B 2 1.134668 0.947504 0.770471 11.00000 -1.20000
AFIX 0
C47 1 0.757080 1.014094 0.829673 11.00000 0.03838 0.05540 =
0.02587 -0.01968 0.00684 -0.01271
AFIX 23
H47A 2 0.840538 1.002593 0.853300 11.00000 -1.20000
H47B 2 0.679338 1.029627 0.854784 11.00000 -1.20000
AFIX 0
C49 1 0.802539 0.896399 0.786361 11.00000 0.04061 0.03821 =
0.01847 0.00429 -0.00490 -0.00686
AFIX 13
H49A 2 0.758581 0.849061 0.786893 11.00000 -1.20000
AFIX 0
C44 1 0.967961 0.996357 0.729643 11.00000 0.02065 0.04319 =
0.02367 -0.01298 0.00217 -0.01325
AFIX 13
H44A 2 1.034171 1.003158 0.697217 11.00000 -1.20000
AFIX 0
C42 1 0.956557 0.897687 0.802293 11.00000 0.04408 0.05112 =
0.02745 -0.00606 -0.01230 0.00904
AFIX 23
H42A 2 1.003076 0.855352 0.787393 11.00000 -1.20000
H42B 2 0.964197 0.896342 0.843751 11.00000 -1.20000
AFIX 0
C41 1 1.247520 0.981921 0.587327 11.00000 0.03733 0.11286 =
0.07690 -0.02708 0.00176 -0.03739
AFIX 33
H41A 2 1.257609 1.016774 0.557571 11.00000 -1.50000
H41B 2 1.332970 0.952737 0.588501 11.00000 -1.50000
H41C 2 1.235398 1.005332 0.623571 11.00000 -1.50000
HKLF 4
REM ljh149 in P2(1)2(1)2(1)
REM R1 = 0.0218 for 8788 Fo > 4sig(Fo) and 0.0234 for all 9076 data
REM 496 parameters refined using 0 restraints
END
WGHT 0.0297 2.3785
REM Highest difference peak 0.841, deepest hole -0.907, 1-sigma level 0.080
Q1 1 1.3609 0.9979 0.4404 11.00000 0.05 0.84
Q2 1 0.7049 0.9582 0.6635 11.00000 0.05 0.76
Q3 1 0.7374 0.9912 0.6934 11.00000 0.05 0.61
Q4 1 0.8291 0.9568 0.7412 11.00000 0.05 0.59
Q5 1 0.4042 1.0595 0.9005 11.00000 0.05 0.55
Q6 1 0.8277 0.9584 0.6649 11.00000 0.05 0.48
Q7 1 0.6997 0.9572 0.7468 11.00000 0.05 0.46
Q8 1 0.7922 0.8973 0.7291 11.00000 0.05 0.41
Q9 1 0.8648 0.9158 0.7086 11.00000 0.05 0.40
Q10 1 0.7606 1.5024 0.5698 11.00000 0.05 0.37
;