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_7021310
_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 P O3 Rh, C4 H10 O'
_chemical_formula_sum            'C53 H49 Cl O4 P Rh'
_chemical_formula_weight         919.25
_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                   9.5919(3)
_cell_length_b                   19.2348(5)
_cell_length_c                   23.6141(6)
_cell_measurement_reflns_used    11308
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4719
_cell_measurement_theta_min      2.9933
_cell_volume                     4356.8(2)
_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 0.895
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25484
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.9002
_exptl_absorpt_correction_T_min  0.8139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Fri Jun 17 15:05:29 2011'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+2.1824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                8683
_reflns_number_total             9385
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50482d.txt
_cod_data_source_block           ljh97_3a
_cod_database_code               7021310
_computing_special_details
;
TITL ljh97 in P2(1)2(1)2(1)
CELL 0.71073 9.5919 19.2348 23.6141 90.000 90.000 90.000
ZERR 4.00 0.0003 0.0005 0.0006 0.000 0.000 0.000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H O P CL RH
UNIT 212 196 16 4 4 4
TEMP -123
L.S. 8
BOND $H
CONF
FMAP 2
PLAN 5
SIZE 0.40 0.20 0.20
ACTA 50
REM EXTI 0.000000
WGHT 0.034300 2.182400
FVAR 0.24702
RH 6 0.730249 0.449885 0.789821 11.00000 0.02237 0.02200 =
0.01427 0.00122 -0.00101 0.00473
CL 5 0.932151 0.388268 0.818008 11.00000 0.02526 0.02712 =
0.02109 -0.00157 -0.00202 0.00845
P 4 0.722833 0.483588 0.879296 11.00000 0.01811 0.01770 =
0.01557 0.00134 -0.00012 0.00115
O1 3 0.865208 0.523384 0.898556 11.00000 0.01933 0.01874 =
0.01973 0.00195 -0.00001 -0.00078
O2 3 0.607918 0.543657 0.892054 11.00000 0.01975 0.01874 =
0.02057 -0.00274 0.00083 0.00115
O3 3 0.371883 0.432356 0.912052 11.00000 0.02519 0.04120 =
0.04357 0.00324 -0.00605 0.00201
O4 3 0.237259 0.513216 1.068548 11.00000 0.04987 0.05526 =
0.23177 0.03807 -0.01363 0.00317
C1 1 0.886534 0.587404 0.871969 11.00000 0.01992 0.02255 =
0.01610 0.00159 0.00024 -0.00437
C2 1 0.977893 0.589026 0.825416 11.00000 0.02089 0.03134 =
0.02117 -0.00097 0.00231 0.00092
AFIX 43
H2A 2 1.024218 0.548163 0.812905 11.00000 -1.20000
AFIX 0
C3 1 0.997713 0.650787 0.798971 11.00000 0.01988 0.03581 =
0.01892 0.00278 0.00518 -0.00456
AFIX 43
H3A 2 1.060706 0.653269 0.767993 11.00000 -1.20000
AFIX 0
C4 1 0.927232 0.711308 0.816300 11.00000 0.02266 0.02784 =
0.01595 0.00398 -0.00395 -0.00649
C5 1 0.946691 0.775704 0.787603 11.00000 0.02025 0.03671 =
0.01842 0.00727 -0.00265 -0.01189
AFIX 43
H5A 2 1.008750 0.778140 0.756313 11.00000 -1.20000
AFIX 0
C6 1 0.877641 0.833460 0.804473 11.00000 0.02767 0.02882 =
0.02783 0.01412 -0.01104 -0.01037
AFIX 43
H6A 2 0.892349 0.876149 0.785143 11.00000 -1.20000
AFIX 0
C7 1 0.784190 0.830858 0.850416 11.00000 0.03150 0.02249 =
0.02778 0.00533 -0.01049 -0.00211
AFIX 43
H7A 2 0.736453 0.871761 0.861924 11.00000 -1.20000
AFIX 0
C8 1 0.761946 0.769988 0.878415 11.00000 0.02451 0.02554 =
0.02151 0.00204 -0.00154 -0.00218
AFIX 43
H8A 2 0.696572 0.768530 0.908614 11.00000 -1.20000
AFIX 0
C9 1 0.834770 0.708982 0.863163 11.00000 0.02075 0.02317 =
0.01834 0.00335 -0.00309 -0.00605
C10 1 0.817748 0.643927 0.892064 11.00000 0.02251 0.02528 =
0.01392 0.00105 0.00081 -0.00388
C11 1 0.723830 0.634880 0.942009 11.00000 0.02511 0.01671 =
0.01875 0.00186 0.00385 0.00062
C12 1 0.740355 0.673907 0.993283 11.00000 0.02594 0.01715 =
0.01875 0.00247 0.00384 0.00148
C13 1 0.848849 0.722391 1.001568 11.00000 0.03524 0.02207 =
0.01948 0.00180 0.00208 -0.00326
AFIX 43
H13A 2 0.913915 0.730280 0.971926 11.00000 -1.20000
AFIX 0
C14 1 0.862530 0.758121 1.050995 11.00000 0.04287 0.02680 =
0.02733 0.00083 -0.00222 -0.00863
AFIX 43
H14A 2 0.937197 0.790049 1.055712 11.00000 -1.20000
AFIX 0
C15 1 0.765404 0.747721 1.095455 11.00000 0.05275 0.03211 =
0.01991 -0.00453 0.00071 -0.00274
AFIX 43
H15A 2 0.772686 0.773872 1.129454 11.00000 -1.20000
AFIX 0
C16 1 0.662804 0.700581 1.089220 11.00000 0.04238 0.02908 =
0.01956 0.00200 0.01134 0.00838
AFIX 43
H16A 2 0.599467 0.693321 1.119578 11.00000 -1.20000
AFIX 0
C17 1 0.646276 0.661491 1.038889 11.00000 0.03335 0.02116 =
0.02080 0.00363 0.00515 0.00469
C18 1 0.542450 0.610414 1.033378 11.00000 0.02832 0.02420 =
0.02334 0.00241 0.01194 0.00256
AFIX 43
H18A 2 0.478850 0.603016 1.063623 11.00000 -1.20000
AFIX 0
C19 1 0.531196 0.571259 0.985464 11.00000 0.02437 0.01982 =
0.02652 0.00126 0.00757 0.00109
AFIX 43
H19A 2 0.462340 0.535950 0.982458 11.00000 -1.20000
AFIX 0
C20 1 0.623756 0.584361 0.940696 11.00000 0.01964 0.01896 =
0.01761 0.00086 0.00318 0.00269
C21 1 0.709995 0.424756 0.938890 11.00000 0.02233 0.01924 =
0.01540 -0.00026 0.00192 0.00062
C22 1 0.788954 0.439192 0.988255 11.00000 0.02456 0.01908 =
0.02006 -0.00424 -0.00061 -0.00280
AFIX 43
H22A 2 0.849522 0.478262 0.988882 11.00000 -1.20000
AFIX 0
C23 1 0.778976 0.397816 1.034627 11.00000 0.03182 0.02899 =
0.01347 -0.00187 -0.00357 -0.00117
AFIX 43
H23A 2 0.834104 0.407890 1.067026 11.00000 -1.20000
AFIX 0
C24 1 0.688799 0.340483 1.035584 11.00000 0.02065 0.02452 =
0.01778 -0.00002 0.00037 -0.00059
C25 1 0.675588 0.297529 1.083711 11.00000 0.03827 0.03630 =
0.01708 0.00420 -0.00210 -0.00438
AFIX 43
H25A 2 0.730283 0.306990 1.116353 11.00000 -1.20000
AFIX 0
C26 1 0.585934 0.242858 1.084140 11.00000 0.03811 0.04125 =
0.02375 0.01285 -0.00032 -0.00787
AFIX 43
H26A 2 0.577200 0.214884 1.117105 11.00000 -1.20000
AFIX 0
C27 1 0.506497 0.227788 1.036014 11.00000 0.03128 0.03668 =
0.02991 0.01116 -0.00289 -0.01487
AFIX 43
H27A 2 0.444813 0.189150 1.036437 11.00000 -1.20000
AFIX 0
C28 1 0.516273 0.267531 0.988773 11.00000 0.03002 0.03984 =
0.02280 0.00862 -0.00431 -0.01086
AFIX 43
H28A 2 0.460917 0.256534 0.956638 11.00000 -1.20000
AFIX 0
C29 1 0.607870 0.325218 0.986666 11.00000 0.02222 0.02676 =
0.01711 0.00434 0.00004 -0.00275
C30 1 0.621496 0.368584 0.937464 11.00000 0.01955 0.02351 =
0.01829 0.00169 -0.00020 0.00022
C31 1 0.536719 0.348847 0.886519 11.00000 0.02495 0.02875 =
0.01812 0.00772 -0.00543 -0.00560
C32 1 0.580547 0.292104 0.851846 11.00000 0.02561 0.02811 =
0.01865 0.00481 -0.00311 -0.01030
C33 1 0.708329 0.258208 0.858949 11.00000 0.03332 0.02928 =
0.02489 0.00495 -0.00520 -0.00560
AFIX 43
H33A 2 0.769192 0.273068 0.888287 11.00000 -1.20000
AFIX 0
C34 1 0.748029 0.204459 0.824974 11.00000 0.04185 0.03452 =
0.03359 -0.00161 0.00334 -0.00193
AFIX 43
H34A 2 0.836188 0.182982 0.830461 11.00000 -1.20000
AFIX 0
C35 1 0.659090 0.180722 0.781898 11.00000 0.05351 0.03855 =
0.03791 -0.01017 0.00791 -0.00919
AFIX 43
H35A 2 0.686361 0.142885 0.758534 11.00000 -1.20000
AFIX 0
C36 1 0.535415 0.211745 0.773903 11.00000 0.04709 0.04760 =
0.02140 -0.00739 -0.00187 -0.01972
AFIX 43
H36A 2 0.476271 0.195548 0.744453 11.00000 -1.20000
AFIX 0
C37 1 0.490323 0.268038 0.808134 11.00000 0.03136 0.04060 =
0.02049 0.00813 -0.00682 -0.01458
C38 1 0.362651 0.300371 0.800559 11.00000 0.03511 0.05074 =
0.02315 0.00352 -0.00950 -0.01619
AFIX 43
H38A 2 0.302097 0.283875 0.771699 11.00000 -1.20000
AFIX 0
C39 1 0.321240 0.354726 0.832921 11.00000 0.02111 0.04965 =
0.03128 0.01544 -0.00864 -0.00484
AFIX 43
H39A 2 0.233713 0.376350 0.826274 11.00000 -1.20000
AFIX 0
C40 1 0.409369 0.379050 0.876710 11.00000 0.02554 0.02894 =
0.02893 0.00690 -0.00101 -0.00442
C41 1 0.250607 0.470751 0.897595 11.00000 0.03597 0.07493 =
0.06947 -0.00859 -0.00612 0.02334
AFIX 33
H41A 2 0.234706 0.507030 0.926008 11.00000 -1.50000
H41B 2 0.170028 0.439458 0.896459 11.00000 -1.50000
H41C 2 0.263364 0.492271 0.860336 11.00000 -1.50000
AFIX 0
C42 1 0.705876 0.389086 0.709744 11.00000 0.04112 0.03878 =
0.01354 -0.01069 -0.00658 0.01018
AFIX 13
H42A 2 0.753058 0.342727 0.710021 11.00000 -1.20000
AFIX 0
C43 1 0.791435 0.443326 0.698084 11.00000 0.03799 0.04466 =
0.01529 -0.00125 0.00263 0.01695
AFIX 13
H43A 2 0.890951 0.430160 0.691429 11.00000 -1.20000
AFIX 0
C44 1 0.744350 0.506531 0.666375 11.00000 0.03951 0.05251 =
0.02200 0.01159 0.00090 0.00509
AFIX 23
H44A 2 0.664085 0.494094 0.642043 11.00000 -1.20000
H44B 2 0.820796 0.522693 0.641472 11.00000 -1.20000
AFIX 0
C45 1 0.702251 0.565083 0.705757 11.00000 0.04146 0.03703 =
0.02936 0.01724 -0.00273 0.00400
AFIX 23
H45A 2 0.786166 0.592659 0.715310 11.00000 -1.20000
H45B 2 0.636705 0.596128 0.685526 11.00000 -1.20000
AFIX 0
C46 1 0.634529 0.540988 0.759966 11.00000 0.03189 0.02560 =
0.02412 0.00534 -0.00320 0.00788
AFIX 13
H46A 2 0.625199 0.578255 0.789248 11.00000 -1.20000
AFIX 0
C47 1 0.533751 0.488713 0.764119 11.00000 0.02739 0.03451 =
0.02238 0.00577 -0.00258 0.01052
AFIX 13
H47A 2 0.466772 0.495571 0.796087 11.00000 -1.20000
AFIX 0
C48 1 0.471567 0.451094 0.713833 11.00000 0.02862 0.04917 =
0.02902 0.00590 -0.00719 0.00078
AFIX 23
H48A 2 0.464876 0.484066 0.681756 11.00000 -1.20000
H48B 2 0.375670 0.436354 0.723638 11.00000 -1.20000
AFIX 0
C49 1 0.554577 0.386745 0.694368 11.00000 0.04037 0.04188 =
0.02671 0.00015 -0.00889 -0.00145
AFIX 23
H49A 2 0.512360 0.344746 0.711492 11.00000 -1.20000
H49B 2 0.546211 0.382394 0.652732 11.00000 -1.20000
AFIX 0
C50 1 0.281200 0.441717 1.080993 11.00000 0.12433 0.10219 =
0.27637 0.13479 0.05133 0.02318
AFIX 23
H50A 2 0.210352 0.417268 1.104076 11.00000 -1.20000
H50B 2 0.297115 0.415200 1.045647 11.00000 -1.20000
AFIX 0
C51 1 0.400936 0.449738 1.110140 11.00000 0.04142 0.12897 =
0.55873 0.22728 -0.08088 -0.03522
AFIX 33
H51A 2 0.422815 0.406551 1.130285 11.00000 -1.50000
H51B 2 0.390309 0.487674 1.137505 11.00000 -1.50000
H51C 2 0.476745 0.460822 1.083823 11.00000 -1.50000
AFIX 0
C52 1 0.117954 0.512738 1.043481 11.00000 0.04844 0.10042 =
0.06812 -0.03243 0.00787 -0.02248
AFIX 23
H52A 2 0.043716 0.499729 1.070611 11.00000 -1.20000
H52B 2 0.118358 0.478380 1.012266 11.00000 -1.20000
AFIX 0
C53 1 0.090368 0.586879 1.019658 11.00000 0.08566 0.06843 =
0.08791 -0.01487 -0.02896 0.02048
AFIX 33
H53A 2 0.001890 0.587170 0.998907 11.00000 -1.50000
H53B 2 0.166293 0.600021 0.994034 11.00000 -1.50000
H53C 2 0.085544 0.620151 1.051027 11.00000 -1.50000
HKLF 4
REM ljh97 in P2(1)2(1)2(1)
REM R1 = 0.0330 for 8683 Fo > 4sig(Fo) and 0.0388 for all 9385 data
REM 541 parameters refined using 0 restraints
END
WGHT 0.0343 2.1884
REM Highest difference peak 0.745, deepest hole -0.497, 1-sigma level 0.067
Q1 1 0.7075 0.5445 0.7971 11.00000 0.05 0.75
Q2 1 0.3760 0.4605 1.1613 11.00000 0.05 0.54
Q3 1 0.1249 0.4574 1.0576 11.00000 0.05 0.52
Q4 1 0.3648 0.4137 1.0611 11.00000 0.05 0.48
Q5 1 0.2883 0.4509 1.1075 11.00000 0.05 0.44
;