MOP-phosphonites: A novel ligand class for asymmetric catalysis.
Ficks, Arne; Hiney, Rachel M.; Harrington, Ross W.; Gilheany, Declan G.; Higham, Lee J.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3515–3522; doi:10.1039/c2dt12214f

data_7018613
_publ_section_title
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 MOP-phosphonites: A novel ligand class for asymmetric catalysis.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3515
_journal_page_last               3522
_journal_paper_doi               10.1039/c2dt12214f
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H34 Cl O3 P Pd, C H2 Cl2'
_chemical_formula_sum            'C46 H36 Cl3 O3 P Pd'
_chemical_formula_weight         880.47
_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                   10.4065(4)
_cell_length_b                   17.4563(4)
_cell_length_c                   21.7841(5)
_cell_measurement_reflns_used    8935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5193
_cell_measurement_theta_min      2.9421
_cell_volume                     3957.3(2)
_computing_cell_refinement
;
'Thu Nov 10 20:28:29 2011'
;
_computing_data_collection
;
'Thu Nov 10 20:28:29 2011'
;
_computing_data_reduction
;
'Thu Nov 10 20:28:29 2011'
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.868
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22011
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.8639
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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'Thu Nov 10 20:28:29 2011'
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.538
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8320
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0493P)^2^+0.1841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                7461
_reflns_number_total             8320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt12214f.txt
_cod_data_source_block           ljh146
_cod_database_code               7018613
_computing_special_details
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TITL ljh146 in P2(1)2(1)2(1)
CELL 0.71073 10.4065 17.4563 21.7841 90.000 90.000 90.000
ZERR 4.00 0.0004 0.0004 0.0005 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 PD Cl
UNIT 184 144 12 4 4 12
TEMP -123

REM 1 DCM molecule squeezed per AU

L.S. 8
BOND $H
CONF
ACTA 50

FMAP 2
PLAN 5

REM colourless block
SIZE 0.32 0.20 0.20

SIMU C42 > C45
DELU c42 > c45

OMIT 0 2 3
OMIT 1 0 3
OMIT 2 0 2

REM EXTI 0.000064
WGHT 0.049300 0.184100
FVAR 1.56575 0.52356
PD 5 0.810274 0.721039 0.840306 11.00000 0.03889 0.03363 =
0.02863 0.01182 -0.00438 -0.00574
CL1 6 1.022711 0.768668 0.851955 11.00000 0.04193 0.06335 =
0.03981 0.01317 -0.00949 -0.01443
P 4 0.772362 0.791953 0.756752 11.00000 0.02916 0.02360 =
0.02284 0.00412 0.00232 -0.00008
O1 3 0.885363 0.780222 0.706152 11.00000 0.02646 0.02687 =
0.02494 0.00119 0.00214 0.00011
O2 3 0.647411 0.764967 0.717628 11.00000 0.02829 0.02625 =
0.02361 0.00382 0.00101 0.00032
O3 3 0.427930 0.877234 0.778476 11.00000 0.03504 0.05022 =
0.06631 0.00169 0.01677 -0.00704
C1 1 0.888110 0.705995 0.681265 11.00000 0.02599 0.03032 =
0.02479 0.00221 0.00329 -0.00120
C2 1 0.973616 0.653503 0.705712 11.00000 0.02988 0.04398 =
0.02962 0.00516 0.00015 0.00485
AFIX 43
H2A 2 1.029999 0.667813 0.738036 11.00000 -1.20000
AFIX 0
C3 1 0.975618 0.580309 0.682451 11.00000 0.03582 0.03180 =
0.03635 0.00887 0.00076 0.01116
AFIX 43
H3A 2 1.033878 0.543696 0.698773 11.00000 -1.20000
AFIX 0
C4 1 0.892167 0.559365 0.634767 11.00000 0.03473 0.03061 =
0.03223 0.00904 0.01007 0.00355
C5 1 0.892377 0.483870 0.611263 11.00000 0.05275 0.03262 =
0.04484 0.00391 0.00936 0.00472
AFIX 43
H5A 2 0.949577 0.447091 0.628190 11.00000 -1.20000
AFIX 0
C6 1 0.812757 0.463013 0.565168 11.00000 0.06755 0.03412 =
0.05708 -0.00995 0.00115 0.00155
AFIX 43
H6A 2 0.816852 0.412597 0.548863 11.00000 -1.20000
AFIX 0
C7 1 0.725504 0.514934 0.541778 11.00000 0.08774 0.05101 =
0.06279 -0.02065 -0.02947 0.00945
AFIX 43
H7A 2 0.668891 0.499403 0.509911 11.00000 -1.20000
AFIX 0
C8 1 0.718898 0.589151 0.563840 11.00000 0.06912 0.04503 =
0.04552 -0.01373 -0.02032 0.01589
AFIX 43
H8A 2 0.656737 0.623624 0.547811 11.00000 -1.20000
AFIX 0
C9 1 0.803810 0.613552 0.609817 11.00000 0.03728 0.03153 =
0.02794 0.00046 0.00333 0.00529
C10 1 0.804171 0.690318 0.633911 11.00000 0.03361 0.02862 =
0.02286 0.00407 0.00453 0.00690
C11 1 0.714502 0.751494 0.613242 11.00000 0.02963 0.02674 =
0.02748 0.00210 -0.00628 0.00501
C12 1 0.707766 0.777595 0.551213 11.00000 0.04081 0.03867 =
0.02509 0.00255 -0.00368 0.00487
C13 1 0.792364 0.749794 0.504882 11.00000 0.07129 0.05944 =
0.02904 0.00733 -0.00334 0.02135
AFIX 43
H13A 2 0.854479 0.711831 0.514675 11.00000 -1.20000
AFIX 0
C14 1 0.784359 0.777560 0.446521 11.00000 0.09310 0.07440 =
0.02645 0.01216 0.00304 0.03343
AFIX 43
H14A 2 0.839941 0.757570 0.415858 11.00000 -1.20000
AFIX 0
C15 1 0.696132 0.834871 0.430667 11.00000 0.08676 0.09300 =
0.02938 0.01721 -0.00889 0.03012
AFIX 43
H15A 2 0.692872 0.853643 0.389764 11.00000 -1.20000
AFIX 0
C16 1 0.614420 0.863845 0.474339 11.00000 0.05791 0.06301 =
0.03654 0.01477 -0.00986 0.01627
AFIX 43
H16A 2 0.554644 0.902698 0.463518 11.00000 -1.20000
AFIX 0
C17 1 0.618663 0.836050 0.535753 11.00000 0.03945 0.04260 =
0.03561 0.00916 -0.00732 0.00772
C18 1 0.541949 0.868770 0.581865 11.00000 0.03008 0.03513 =
0.04226 0.00531 -0.00518 0.00517
AFIX 43
H18A 2 0.481972 0.907682 0.571442 11.00000 -1.20000
AFIX 0
C19 1 0.552322 0.845613 0.640939 11.00000 0.02730 0.03230 =
0.04064 0.00406 0.00078 0.00316
AFIX 43
H19A 2 0.500752 0.868500 0.671899 11.00000 -1.20000
AFIX 0
C20 1 0.639427 0.787829 0.655971 11.00000 0.02813 0.02772 =
0.02612 0.00498 -0.00646 -0.00553
C21 1 0.759415 0.895398 0.755710 11.00000 0.02960 0.03123 =
0.02390 0.00438 0.00074 -0.00094
C22 1 0.825449 0.938640 0.710727 11.00000 0.03945 0.02903 =
0.02292 0.00011 0.00695 -0.00199
AFIX 43
H22A 2 0.884461 0.913779 0.684077 11.00000 -1.20000
AFIX 0
C23 1 0.805519 1.015419 0.705138 11.00000 0.03755 0.03098 =
0.03076 0.00565 0.00040 -0.00829
AFIX 43
H23A 2 0.851125 1.043841 0.674998 11.00000 -1.20000
AFIX 0
C24 1 0.717333 1.052714 0.744016 11.00000 0.02367 0.02811 =
0.03269 0.00144 -0.00621 -0.00273
C25 1 0.695749 1.133323 0.739363 11.00000 0.03077 0.02835 =
0.05034 0.00486 -0.00580 -0.00024
AFIX 43
H25A 2 0.740677 1.162435 0.709413 11.00000 -1.20000
AFIX 0
C26 1 0.611139 1.168517 0.777643 11.00000 0.03295 0.02865 =
0.07462 0.00315 -0.00305 0.00928
AFIX 43
H26A 2 0.596031 1.221984 0.773894 11.00000 -1.20000
AFIX 0
C27 1 0.546524 1.126420 0.822349 11.00000 0.04250 0.03888 =
0.07253 -0.00746 0.01349 0.01115
AFIX 43
H27A 2 0.488785 1.152128 0.849119 11.00000 -1.20000
AFIX 0
C28 1 0.563784 1.049052 0.828849 11.00000 0.04110 0.03309 =
0.05664 0.00276 0.01325 0.00614
AFIX 43
H28A 2 0.517541 1.021560 0.859319 11.00000 -1.20000
AFIX 0
C29 1 0.651678 1.010110 0.789534 11.00000 0.02798 0.02693 =
0.03588 0.00121 0.00412 0.00268
C30 1 0.674164 0.930003 0.794982 11.00000 0.03264 0.02741 =
0.02964 0.00445 0.00544 -0.00175
C31 1 0.603188 0.886806 0.844190 11.00000 0.05239 0.03047 =
0.04027 0.00707 0.02614 0.00607
C32 1 0.662142 0.876069 0.903121 11.00000 0.06518 0.06110 =
0.03944 0.01555 0.02304 0.01136
C33 1 0.785959 0.904053 0.917631 11.00000 0.06460 0.11329 =
0.04478 0.02913 0.01419 0.01339
AFIX 43
H33A 2 0.835169 0.928736 0.886680 11.00000 -1.20000
AFIX 0
C34 1 0.835842 0.896433 0.974631 11.00000 0.08350 0.19662 =
0.04004 0.02948 0.00768 0.00512
AFIX 43
H34A 2 0.918089 0.916828 0.984170 11.00000 -1.20000
AFIX 0
C35 1 0.762245 0.857014 1.020335 11.00000 0.12184 0.20068 =
0.04090 0.04782 0.02091 0.03322
AFIX 43
H35A 2 0.797349 0.850750 1.060277 11.00000 -1.20000
AFIX 0
C36 1 0.645388 0.828768 1.008310 11.00000 0.09777 0.13738 =
0.05105 0.04509 0.03530 0.01455
AFIX 43
H36A 2 0.599472 0.801907 1.039252 11.00000 -1.20000
AFIX 0
C37 1 0.591448 0.838688 0.950808 11.00000 0.07712 0.07322 =
0.05211 0.02238 0.03417 0.01122
C38 1 0.467687 0.812970 0.937465 11.00000 0.09723 0.05613 =
0.07007 0.02885 0.05175 0.01332
AFIX 43
H38A 2 0.421355 0.786706 0.968593 11.00000 -1.20000
AFIX 0
C39 1 0.409349 0.823760 0.881420 11.00000 0.05627 0.04380 =
0.08413 0.00625 0.04079 0.00263
AFIX 43
H39A 2 0.324485 0.805880 0.874138 11.00000 -1.20000
AFIX 0
C40 1 0.479534 0.862419 0.834655 11.00000 0.05713 0.03132 =
0.05536 0.00326 0.02663 0.00119
C41 1 0.290895 0.870877 0.771788 11.00000 0.04677 0.08063 =
0.09177 0.00475 0.02331 0.01182
AFIX 137
H41A 2 0.265885 0.887603 0.730540 11.00000 -1.50000
H41B 2 0.248466 0.903255 0.802445 11.00000 -1.50000
H41C 2 0.264931 0.817441 0.777822 11.00000 -1.50000
AFIX 0
C42 1 0.630387 0.666531 0.846233 11.00000 0.05205 0.04318 =
0.05241 0.00824 0.00366 -0.01419
AFIX 23
H42A 2 0.570171 0.686817 0.877436 11.00000 -1.20000
H42B 2 0.588219 0.653690 0.806817 11.00000 -1.20000
AFIX 0
C43 1 0.724282 0.614255 0.867456 11.00000 0.05388 0.03654 =
0.08297 0.03029 0.00508 -0.00686
C44 1 0.799256 0.638961 0.915875 11.00000 0.07101 0.10449 =
0.08068 0.07579 -0.01636 -0.02368
AFIX 23
H44A 2 0.877880 0.608945 0.924596 11.00000 -1.20000
H44B 2 0.753222 0.655962 0.953240 11.00000 -1.20000
AFIX 0
C45 1 0.753406 0.544732 0.828263 11.00000 0.11713 0.03644 =
0.21994 0.00011 0.05616 -0.00570
AFIX 137
H45A 2 0.691533 0.504024 0.837540 11.00000 -1.50000
H45B 2 0.840581 0.526591 0.837109 11.00000 -1.50000
H45C 2 0.746949 0.558595 0.784778 11.00000 -1.50000

HKLF 4

REM ljh146 in P2(1)2(1)2(1)
REM R1 = 0.0385 for 7461 Fo > 4sig(Fo) and 0.0455 for all 8320 data
REM 463 parameters refined using 24 restraints

END

WGHT 0.0493 0.1841
REM Highest difference peak 0.380, deepest hole -0.538, 1-sigma level 0.067
Q1 1 0.8043 0.6949 0.8009 11.00000 0.05 0.38
Q2 1 0.8729 0.3985 0.8890 11.00000 0.05 0.37
Q3 1 0.8360 0.6784 0.8266 11.00000 0.05 0.36
Q4 1 0.7411 0.7797 0.8386 11.00000 0.05 0.35
Q5 1 0.4229 0.5607 0.4613 11.00000 0.05 0.31
;