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_7021311
_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         'C82 H54 O6 P2 Rh +, B F4 -, 2 C4 H10 O'
_chemical_formula_sum            'C90 H74 B F4 O8 P2 Rh'
_chemical_formula_weight         1535.15
_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                   14.0434(4)
_cell_length_b                   20.3321(6)
_cell_length_c                   25.7605(6)
_cell_measurement_reflns_used    19157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.4304
_cell_measurement_theta_min      1.7133
_cell_volume                     7355.4(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36016
_diffrn_reflns_theta_full        54.24
_diffrn_reflns_theta_max         54.24
_diffrn_reflns_theta_min         7.67
_exptl_absorpt_coefficient_mu    2.864
_exptl_absorpt_correction_T_max  0.8700
_exptl_absorpt_correction_T_min  0.5981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Thu Jan 13 11:41:54 2011'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.037(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         8935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+3.0906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                8181
_reflns_number_total             8935
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50482d.txt
_cod_data_source_block           ljh71_4b
_cod_database_code               7021311
_computing_special_details
;
TITL ljh71 in P2(1)2(1)2(1)
CELL 1.54178 14.0434 20.3321 25.7605 90.000 90.000 90.000
ZERR 4.00 0.0004 0.0006 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 B O F P RH
UNIT 360 296 4 32 16 8 4
TEMP -123
L.S. 8
BOND $H
CONF
SIZE 0.20 0.05 0.05
FMAP 2
PLAN 5
SHEL 5.8 0.95
ACTA
REM EXTI 0.000000
WGHT 0.062500 3.090600
FVAR 1.03509
RH1 7 0.879706 0.392397 0.882799 11.00000 0.02692 0.02172 =
0.03292 -0.00134 -0.00076 0.00180
P1 6 0.765041 0.329756 0.850579 11.00000 0.02915 0.02247 =
0.02450 0.00025 0.00136 0.00128
P2 6 0.786552 0.473809 0.905326 11.00000 0.02695 0.02564 =
0.02842 -0.00088 -0.00134 0.00090
O1 4 0.751406 0.328988 0.788486 11.00000 0.03127 0.02553 =
0.02841 0.00069 0.00387 0.00299
O2 4 0.662122 0.356611 0.869406 11.00000 0.02717 0.02730 =
0.02824 -0.00123 -0.00188 -0.00078
O3 4 0.650120 0.200318 0.753762 11.00000 0.03887 0.03920 =
0.03657 -0.00378 -0.00886 -0.00173
O4 4 0.712389 0.477143 0.953352 11.00000 0.03006 0.03362 =
0.02965 0.00368 -0.00329 0.00427
O5 4 0.723349 0.502107 0.857619 11.00000 0.03161 0.02626 =
0.02588 -0.00232 0.00273 0.00326
O6 4 0.995805 0.420621 0.992336 11.00000 0.04720 0.03409 =
0.03768 0.00682 -0.01224 -0.00418
O7 4 0.357702 0.900756 0.904494 11.00000 0.28521 0.04893 =
0.11419 0.01531 -0.06559 -0.01838
O8 4 1.040346 0.424298 0.607073 11.00000 0.13334 0.05299 =
0.04210 0.00331 -0.01858 -0.01177
B1 3 0.701156 0.287888 1.075302 11.00000 0.05493 0.03808 =
0.02657 0.00100 -0.00969 -0.00853
F1 5 0.766062 0.277668 1.037837 11.00000 0.20968 0.16487 =
0.06282 -0.03668 0.06280 -0.08948
F2 5 0.728258 0.342735 1.099254 11.00000 0.11885 0.08993 =
0.17241 -0.07474 0.06378 -0.04332
F3 5 0.611182 0.294370 1.060521 11.00000 0.08981 0.13706 =
0.29707 0.16610 -0.11347 -0.06708
F4 5 0.703801 0.236588 1.109890 11.00000 0.05416 0.08961 =
0.09911 0.04875 -0.00796 -0.00010
C1 1 0.723614 0.390363 0.767530 11.00000 0.03459 0.02544 =
0.02866 0.00513 0.00160 0.00362
C2 1 0.795400 0.427267 0.743204 11.00000 0.03155 0.03565 =
0.03551 -0.00197 0.00429 -0.00259
AFIX 43
H2A 2 0.858832 0.411200 0.741357 11.00000 -1.20000
AFIX 0
C3 1 0.771882 0.486807 0.722259 11.00000 0.04942 0.04102 =
0.03378 0.01278 0.01024 -0.00626
AFIX 43
H3A 2 0.819531 0.512307 0.705522 11.00000 -1.20000
AFIX 0
C4 1 0.678344 0.510868 0.725103 11.00000 0.04978 0.02973 =
0.03160 -0.00286 0.00711 0.00050
C5 1 0.653109 0.574396 0.703114 11.00000 0.07070 0.02780 =
0.03894 0.01273 0.00389 -0.00141
AFIX 43
H5A 2 0.699924 0.599412 0.685259 11.00000 -1.20000
AFIX 0
C6 1 0.563926 0.598096 0.707835 11.00000 0.07182 0.02637 =
0.03998 0.00677 -0.00555 0.00456
AFIX 43
H6A 2 0.548000 0.639219 0.692631 11.00000 -1.20000
AFIX 0
C7 1 0.494567 0.562560 0.734983 11.00000 0.04684 0.03871 =
0.03993 -0.00434 0.00073 0.00969
AFIX 43
H7A 2 0.432527 0.580536 0.738834 11.00000 -1.20000
AFIX 0
C8 1 0.514662 0.502321 0.756080 11.00000 0.03605 0.02094 =
0.03617 -0.00107 -0.00638 0.00505
AFIX 43
H8A 2 0.466619 0.479421 0.774717 11.00000 -1.20000
AFIX 0
C9 1 0.605989 0.473657 0.750527 11.00000 0.04648 0.02446 =
0.02317 -0.00071 -0.00508 -0.00074
C10 1 0.630784 0.409048 0.770709 11.00000 0.02819 0.02246 =
0.02590 0.00039 -0.00292 -0.00228
C11 1 0.558858 0.365501 0.795861 11.00000 0.03127 0.02307 =
0.02700 -0.00088 0.00498 0.00667
C12 1 0.468317 0.347887 0.772514 11.00000 0.02814 0.02529 =
0.02800 -0.00936 -0.00031 0.00868
C13 1 0.442517 0.367683 0.721682 11.00000 0.03913 0.02330 =
0.04013 -0.00447 -0.00167 0.00893
AFIX 43
H13A 2 0.487386 0.390117 0.700513 11.00000 -1.20000
AFIX 0
C14 1 0.353728 0.354721 0.703003 11.00000 0.03861 0.03023 =
0.03700 -0.00860 -0.01275 0.00787
AFIX 43
H14A 2 0.336459 0.369759 0.669380 11.00000 -1.20000
AFIX 0
C15 1 0.287551 0.319503 0.732726 11.00000 0.03388 0.04658 =
0.05419 -0.01895 -0.00816 0.00962
AFIX 43
H15A 2 0.225163 0.312294 0.719654 11.00000 -1.20000
AFIX 0
C16 1 0.311786 0.295854 0.779619 11.00000 0.03597 0.03504 =
0.04304 -0.00694 0.00648 -0.00382
AFIX 43
H16A 2 0.266940 0.270814 0.798899 11.00000 -1.20000
AFIX 0
C17 1 0.403417 0.307807 0.800669 11.00000 0.02848 0.03335 =
0.03470 -0.00640 0.00400 0.00324
C18 1 0.430209 0.280822 0.848805 11.00000 0.03086 0.03161 =
0.03820 -0.00434 0.00690 -0.00232
AFIX 43
H18A 2 0.387509 0.252848 0.866988 11.00000 -1.20000
AFIX 0
C19 1 0.517262 0.294742 0.869371 11.00000 0.03353 0.02875 =
0.02560 0.00340 0.00391 0.00597
AFIX 43
H19A 2 0.535863 0.275239 0.901311 11.00000 -1.20000
AFIX 0
C20 1 0.579910 0.337903 0.843556 11.00000 0.02542 0.02360 =
0.02850 -0.00420 0.00048 0.00074
C21 1 0.760537 0.242914 0.867510 11.00000 0.02822 0.02236 =
0.03307 -0.00006 -0.00448 0.00228
C22 1 0.738911 0.234326 0.920858 11.00000 0.03867 0.02914 =
0.02658 -0.00200 -0.00287 0.00413
AFIX 43
H22A 2 0.731711 0.271845 0.942484 11.00000 -1.20000
AFIX 0
C23 1 0.728408 0.173738 0.941369 11.00000 0.04511 0.03512 =
0.03120 0.00299 -0.00525 -0.00169
AFIX 43
H23A 2 0.714856 0.169237 0.977324 11.00000 -1.20000
AFIX 0
C24 1 0.737226 0.116883 0.910271 11.00000 0.03714 0.03189 =
0.03715 0.00574 0.00145 0.00113
C25 1 0.723176 0.052832 0.930625 11.00000 0.07888 0.03830 =
0.05487 0.00693 0.01345 -0.00425
AFIX 43
H25A 2 0.706998 0.047425 0.966178 11.00000 -1.20000
AFIX 0
C26 1 0.732613 -0.000556 0.899864 11.00000 0.08767 0.02787 =
0.07197 0.01619 0.02145 -0.00597
AFIX 43
H26A 2 0.724390 -0.043170 0.914309 11.00000 -1.20000
AFIX 0
C27 1 0.754334 0.005815 0.846981 11.00000 0.07430 0.02905 =
0.07415 -0.00895 0.01253 -0.00654
AFIX 43
H27A 2 0.759955 -0.032147 0.825700 11.00000 -1.20000
AFIX 0
C28 1 0.767314 0.066828 0.826349 11.00000 0.04252 0.03330 =
0.04463 -0.00457 0.00510 -0.00842
AFIX 43
H28A 2 0.782111 0.070778 0.790499 11.00000 -1.20000
AFIX 0
C29 1 0.759378 0.124619 0.856841 11.00000 0.02973 0.02417 =
0.04288 -0.00038 0.00361 -0.00502
C30 1 0.773800 0.188864 0.835349 11.00000 0.01858 0.02629 =
0.03275 0.00488 -0.00191 -0.00162
C31 1 0.807916 0.193060 0.780370 11.00000 0.03641 0.02284 =
0.02554 -0.00458 -0.00025 -0.00097
C32 1 0.907239 0.187279 0.770444 11.00000 0.04386 0.02410 =
0.03111 -0.00398 0.00693 -0.00268
C33 1 0.976058 0.177523 0.809841 11.00000 0.03183 0.02992 =
0.03767 -0.00947 0.00249 -0.00392
AFIX 43
H33A 2 0.955618 0.174045 0.844889 11.00000 -1.20000
AFIX 0
C34 1 1.070887 0.172971 0.798940 11.00000 0.03334 0.03878 =
0.04927 -0.01586 -0.00198 -0.00106
AFIX 43
H34A 2 1.115269 0.166939 0.826361 11.00000 -1.20000
AFIX 0
C35 1 1.103316 0.177123 0.747629 11.00000 0.03287 0.04669 =
0.06502 -0.02607 0.01293 -0.00348
AFIX 43
H35A 2 1.169589 0.175585 0.740332 11.00000 -1.20000
AFIX 0
C36 1 1.038928 0.183408 0.708090 11.00000 0.05785 0.03825 =
0.04886 -0.01230 0.02249 -0.00756
AFIX 43
H36A 2 1.061013 0.184505 0.673243 11.00000 -1.20000
AFIX 0
C37 1 0.939986 0.188313 0.718063 11.00000 0.04636 0.03362 =
0.03977 -0.00428 0.00766 0.00403
C38 1 0.871956 0.194699 0.678152 11.00000 0.07009 0.04703 =
0.02970 -0.00071 0.01397 -0.00257
AFIX 43
H38A 2 0.892834 0.196174 0.643094 11.00000 -1.20000
AFIX 0
C39 1 0.776274 0.198844 0.688643 11.00000 0.05824 0.03281 =
0.03338 0.00055 -0.00039 -0.00334
AFIX 43
H39A 2 0.731856 0.202578 0.660985 11.00000 -1.20000
AFIX 0
C40 1 0.744040 0.197565 0.740276 11.00000 0.03671 0.02410 =
0.03420 -0.00180 0.00051 -0.00286
C41 1 0.583028 0.213986 0.713731 11.00000 0.05370 0.03668 =
0.04556 -0.00626 -0.01321 0.00127
AFIX 137
H41A 2 0.519051 0.217035 0.728732 11.00000 -1.50000
H41B 2 0.584516 0.178566 0.687943 11.00000 -1.50000
H41C 2 0.599353 0.255762 0.696973 11.00000 -1.50000
AFIX 0
C42 1 0.616156 0.460025 0.948889 11.00000 0.02850 0.02747 =
0.02355 -0.00152 0.00339 0.00464
C43 1 0.585673 0.405638 0.977525 11.00000 0.04394 0.02821 =
0.02863 -0.00043 0.01049 0.00849
AFIX 43
H43A 2 0.628554 0.382380 0.999355 11.00000 -1.20000
AFIX 0
C44 1 0.492496 0.386689 0.973354 11.00000 0.04646 0.02394 =
0.03967 -0.00049 0.01429 -0.00258
AFIX 43
H44A 2 0.470474 0.350805 0.993694 11.00000 -1.20000
AFIX 0
C45 1 0.428506 0.418561 0.940010 11.00000 0.03941 0.02390 =
0.04174 -0.00700 0.01944 -0.00125
C46 1 0.335237 0.393603 0.929205 11.00000 0.03983 0.02700 =
0.05639 -0.00617 0.02382 -0.00293
AFIX 43
H46A 2 0.312783 0.356039 0.947404 11.00000 -1.20000
AFIX 0
C47 1 0.278277 0.422901 0.893248 11.00000 0.02976 0.03067 =
0.08695 -0.01722 0.00993 -0.00448
AFIX 43
H47A 2 0.217320 0.404881 0.885937 11.00000 -1.20000
AFIX 0
C48 1 0.308513 0.478936 0.867142 11.00000 0.03057 0.04022 =
0.05834 -0.01828 0.00078 0.00822
AFIX 43
H48A 2 0.267588 0.499061 0.842445 11.00000 -1.20000
AFIX 0
C49 1 0.395286 0.505249 0.876354 11.00000 0.02677 0.03272 =
0.03986 -0.00713 0.00100 0.00571
AFIX 43
H49A 2 0.413596 0.544297 0.858733 11.00000 -1.20000
AFIX 0
C50 1 0.458711 0.475986 0.911413 11.00000 0.03195 0.02271 =
0.03348 -0.00996 0.00861 -0.00364
C51 1 0.557000 0.498855 0.919014 11.00000 0.03462 0.02363 =
0.02690 -0.00603 0.00757 0.00145
C52 1 0.591373 0.560740 0.895218 11.00000 0.03164 0.02041 =
0.02518 0.00142 0.00226 -0.00027
C53 1 0.546841 0.623065 0.904649 11.00000 0.03191 0.02733 =
0.02473 0.00167 -0.00554 -0.00398
C54 1 0.468244 0.630447 0.938670 11.00000 0.02757 0.03359 =
0.04054 -0.00942 0.00170 0.00083
AFIX 43
H54A 2 0.443202 0.593017 0.956015 11.00000 -1.20000
AFIX 0
C55 1 0.427965 0.690955 0.946830 11.00000 0.03304 0.03852 =
0.04781 -0.01969 0.00169 -0.00018
AFIX 43
H55A 2 0.376059 0.695074 0.970255 11.00000 -1.20000
AFIX 0
C56 1 0.462495 0.747127 0.920949 11.00000 0.04892 0.02835 =
0.04547 -0.01141 -0.00834 0.00219
AFIX 43
H56A 2 0.431951 0.788397 0.925606 11.00000 -1.20000
AFIX 0
C57 1 0.538467 0.742243 0.889762 11.00000 0.04249 0.02037 =
0.04244 -0.00471 -0.00588 0.00233
AFIX 43
H57A 2 0.563126 0.780797 0.873847 11.00000 -1.20000
AFIX 0
C58 1 0.583268 0.680492 0.879869 11.00000 0.03807 0.03053 =
0.03316 -0.00125 -0.00509 -0.00089
C59 1 0.662329 0.674792 0.847114 11.00000 0.04089 0.02468 =
0.04033 0.00986 0.00495 -0.00360
AFIX 43
H59A 2 0.685793 0.712832 0.829941 11.00000 -1.20000
AFIX 0
C60 1 0.706512 0.615814 0.839275 11.00000 0.03184 0.03383 =
0.03211 0.00778 0.00398 -0.00565
AFIX 43
H60A 2 0.760053 0.612469 0.816890 11.00000 -1.20000
AFIX 0
C61 1 0.671063 0.560539 0.864968 11.00000 0.02754 0.01613 =
0.03390 -0.00203 -0.00367 0.00459
C62 1 0.866442 0.539387 0.927524 11.00000 0.02981 0.02639 =
0.02551 -0.00104 -0.00082 0.00201
C63 1 0.832989 0.601079 0.946384 11.00000 0.02893 0.02936 =
0.03458 -0.00933 -0.00231 0.00126
AFIX 43
H63A 2 0.766679 0.609713 0.948991 11.00000 -1.20000
AFIX 0
C64 1 0.897712 0.647235 0.960541 11.00000 0.04365 0.02796 =
0.03016 -0.00556 0.00141 0.00773
AFIX 43
H64A 2 0.875317 0.688627 0.972526 11.00000 -1.20000
AFIX 0
C65 1 0.997704 0.636330 0.958216 11.00000 0.03712 0.02712 =
0.02886 -0.00291 0.00050 -0.00147
C66 1 1.065759 0.683871 0.973024 11.00000 0.04920 0.02941 =
0.04494 -0.01549 0.00654 0.00059
AFIX 43
H66A 2 1.045071 0.726252 0.983697 11.00000 -1.20000
AFIX 0
C67 1 1.160655 0.669918 0.972247 11.00000 0.03918 0.05316 =
0.06726 -0.02873 0.00060 -0.01407
AFIX 43
H67A 2 1.205412 0.702774 0.981848 11.00000 -1.20000
AFIX 0
C68 1 1.193131 0.606460 0.957150 11.00000 0.03128 0.04669 =
0.06663 -0.01682 0.00589 -0.00028
AFIX 43
H68A 2 1.259244 0.596566 0.957328 11.00000 -1.20000
AFIX 0
C69 1 1.128588 0.559943 0.942418 11.00000 0.03756 0.03809 =
0.05071 -0.01497 0.00751 -0.00330
AFIX 43
H69A 2 1.150864 0.517902 0.931857 11.00000 -1.20000
AFIX 0
C70 1 1.030323 0.572285 0.942384 11.00000 0.03289 0.02689 =
0.03023 -0.00685 0.00266 -0.00004
C71 1 0.961021 0.525120 0.926082 11.00000 0.03300 0.02290 =
0.02704 -0.00160 0.00296 0.00369
C72 1 0.993578 0.459375 0.906718 11.00000 0.01993 0.02367 =
0.03834 -0.00458 -0.00454 0.00309
C73 1 1.018347 0.452438 0.852062 11.00000 0.02171 0.02803 =
0.03580 -0.00504 0.00641 -0.00676
C74 1 1.025871 0.505573 0.817025 11.00000 0.03644 0.03498 =
0.03941 -0.00233 0.00333 0.00190
AFIX 43
H74A 2 1.018116 0.549422 0.829041 11.00000 -1.20000
AFIX 0
C75 1 1.044264 0.493820 0.765984 11.00000 0.03844 0.05651 =
0.04057 -0.00470 0.01327 -0.01017
AFIX 43
H75A 2 1.049493 0.529906 0.742732 11.00000 -1.20000
AFIX 0
C76 1 1.055649 0.429872 0.746957 11.00000 0.05309 0.05558 =
0.04254 -0.01306 0.02292 -0.00781
AFIX 43
H76A 2 1.069778 0.423153 0.711284 11.00000 -1.20000
AFIX 0
C77 1 1.046747 0.377916 0.778759 11.00000 0.03130 0.04925 =
0.05235 -0.02637 0.00394 0.00079
AFIX 43
H77A 2 1.052206 0.334758 0.764945 11.00000 -1.20000
AFIX 0
C78 1 1.029462 0.386202 0.832231 11.00000 0.02510 0.03122 =
0.04975 -0.01254 0.01040 0.00010
C79 1 1.018089 0.332673 0.867733 11.00000 0.02564 0.02999 =
0.05743 -0.01148 0.00319 0.00298
AFIX 13
H79A 2 1.011757 0.287330 0.853097 11.00000 -1.20000
AFIX 0
C80 1 1.010224 0.340390 0.921260 11.00000 0.02780 0.02505 =
0.05485 0.01040 -0.00470 0.00602
AFIX 13
H80A 2 1.000694 0.301239 0.944175 11.00000 -1.20000
AFIX 0
C81 1 1.000875 0.405358 0.941757 11.00000 0.03124 0.02756 =
0.03310 -0.00108 -0.01000 -0.00198
C82 1 0.967167 0.368448 1.028069 11.00000 0.06968 0.05045 =
0.04730 0.00935 -0.00521 -0.00439
AFIX 137
H82A 2 0.961952 0.386383 1.063266 11.00000 -1.50000
H82B 2 1.014937 0.333316 1.027619 11.00000 -1.50000
H82C 2 0.905403 0.350647 1.017293 11.00000 -1.50000
AFIX 0
C83 1 0.206128 0.842595 0.897963 11.00000 0.30031 0.15109 =
0.33697 -0.08395 -0.07123 -0.09468
AFIX 137
H83A 2 0.243305 0.823345 0.869578 11.00000 -1.50000
H83B 2 0.139657 0.847452 0.887033 11.00000 -1.50000
H83C 2 0.209296 0.813735 0.928384 11.00000 -1.50000
AFIX 0
C84 1 0.249056 0.913663 0.912576 11.00000 0.08328 0.13279 =
0.08205 0.01814 -0.02036 0.04771
AFIX 23
H84A 2 0.225156 0.948364 0.888974 11.00000 -1.20000
H84B 2 0.234560 0.925863 0.948932 11.00000 -1.20000
AFIX 0
C85 1 0.389113 0.965810 0.920617 11.00000 0.21665 0.08323 =
0.04949 0.00630 0.00278 -0.08330
AFIX 23
H85A 2 0.360190 1.001036 0.899279 11.00000 -1.20000
H85B 2 0.375929 0.974130 0.957795 11.00000 -1.20000
AFIX 0
C86 1 0.489619 0.958593 0.910516 11.00000 0.27849 0.09629 =
0.07131 -0.00665 0.03973 -0.06790
AFIX 137
H86A 2 0.525410 0.989369 0.932346 11.00000 -1.50000
H86B 2 0.502426 0.968049 0.873872 11.00000 -1.50000
H86C 2 0.509292 0.913460 0.918470 11.00000 -1.50000
AFIX 0
C87 1 1.109483 0.320489 0.614235 11.00000 0.27470 0.04579 =
0.08058 -0.01050 -0.07282 0.00149
AFIX 137
H87A 2 1.143423 0.286058 0.595094 11.00000 -1.50000
H87B 2 1.055682 0.300984 0.632944 11.00000 -1.50000
H87C 2 1.152949 0.341249 0.639081 11.00000 -1.50000
AFIX 0
C88 1 1.073733 0.370734 0.577263 11.00000 0.16988 0.05302 =
0.07136 -0.00248 -0.04568 -0.00755
AFIX 23
H88A 2 1.125540 0.385170 0.553823 11.00000 -1.20000
H88B 2 1.021486 0.352343 0.555933 11.00000 -1.20000
AFIX 0
C89 1 1.008828 0.478058 0.575491 11.00000 0.08103 0.06423 =
0.05077 0.00786 0.00101 -0.00084
AFIX 23
H89A 2 0.953898 0.464191 0.554033 11.00000 -1.20000
H89B 2 1.060726 0.492126 0.551972 11.00000 -1.20000
AFIX 0
C90 1 0.980841 0.533152 0.609553 11.00000 0.09290 0.07760 =
0.05488 -0.00403 -0.00040 0.01058
AFIX 137
H90A 2 0.953575 0.568609 0.588502 11.00000 -1.50000
H90B 2 1.036985 0.549555 0.628069 11.00000 -1.50000
H90C 2 0.933384 0.517867 0.634700 11.00000 -1.50000
HKLF 4
REM ljh71 in P2(1)2(1)2(1)
REM R1 = 0.0401 for 8181 Fo > 4sig(Fo) and 0.0461 for all 8935 data
REM 961 parameters refined using 0 restraints
END
WGHT 0.0625 3.2349
REM Highest difference peak 0.798, deepest hole -0.501, 1-sigma level 0.057
Q1 1 0.3233 0.8817 0.8773 11.00000 0.05 0.80
Q2 1 0.4310 0.8894 0.8944 11.00000 0.05 0.73
Q3 1 0.6017 0.3017 1.0784 11.00000 0.05 0.62
Q4 1 0.7035 0.2191 1.0669 11.00000 0.05 0.51
Q5 1 0.6374 0.2678 1.0357 11.00000 0.05 0.48
;