A comparison of MOP-phosphonite ligands and their applications in Rh(i)- and Pd(ii)-catalysed asymmetric transformations.
Fleming, James T.; Wills, Corinne; Waddell, Paul G.; Harrington, Ross W.; Higham, Lee J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15660–15670; doi:10.1039/c6dt02390h

data_7040543
_publ_section_title
;
 A comparison of MOP-phosphonite ligands and their applications in Rh(i)-
 and Pd(ii)-catalysed asymmetric transformations.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15660
_journal_page_last               15670
_journal_paper_doi               10.1039/c6dt02390h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C68 H50 Cl2 O4 P2 Pd, C H Cl3'
_chemical_formula_sum            'C69 H51 Cl5 O4 P2 Pd'
_chemical_formula_weight         1289.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_audit_creation_date             2014-07-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.54920(12)
_cell_length_b                   17.81230(17)
_cell_length_c                   29.1165(3)
_cell_measurement_reflns_used    23972
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      66.2740
_cell_measurement_theta_min      2.8580
_cell_volume                     5989.78(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   16.00  113.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9707   38.0000  -30.0000 97

  2 omega    9.00   74.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9707  -77.0000  120.0000 65

  3 omega  -20.00    6.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9707  -77.0000  120.0000 26

  4 omega   20.00  114.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -93.0000   -4.5865 94

  5 omega   19.00   57.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000   90.0000 38

  6 omega   21.00   76.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -45.0000  150.0000 55

  7 omega   37.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000 -180.0000 32

  8 omega   51.00   79.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -94.0000  -30.0000 28

  9 omega   28.00   54.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -77.0000  -60.0000 26

 10 omega   22.00   50.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000   30.0000 28

 11 omega   44.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000  -60.0000 25

 12 omega   81.00  118.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000  -60.0000 37

 13 omega  129.00  168.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   30.0000 -120.0000 39

 14 omega   36.00   71.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000    0.0000 35

 15 omega   34.00   65.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000    0.0000 31

 16 omega   43.00   68.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000  -30.0000 25

 17 omega   92.00  117.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000    0.0000 25

 18 omega    8.00   52.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -94.0000  120.0000 44

 19 omega   29.00   76.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -45.0000    0.0000 47

 20 omega   83.00  120.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -77.0000  -60.0000 37

 21 omega   93.00  119.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   61.0000 -150.0000 26

 22 omega   17.00   43.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000  150.0000 26

 23 omega   87.00  124.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  125.0000 -180.0000 37

 24 omega  142.00  167.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  125.0000 -180.0000 25

 25 omega   18.00   66.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000  150.0000 48

 26 omega   39.00  108.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -65.0000 -121.2294 69

 27 omega   49.00   97.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   17.0000  -62.3056 48

 28 omega   49.00   82.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -94.0000 -150.0000 33

 29 omega   10.00   35.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -94.0000 -120.0000 25

 30 omega   76.00  115.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   45.0000   30.0000 39

 31 omega   79.00  109.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -93.0000  -68.5509 30

 32 omega   33.00   59.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -82.0000 -104.9057 26

 33 omega   14.00   57.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -93.0000  -68.5509 43
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0201319000
_diffrn_orient_matrix_UB_12      0.0140529000
_diffrn_orient_matrix_UB_13      0.0515949000
_diffrn_orient_matrix_UB_21      0.1288720000
_diffrn_orient_matrix_UB_22      0.0203070000
_diffrn_orient_matrix_UB_23      0.0058439000
_diffrn_orient_matrix_UB_31      -0.0281085000
_diffrn_orient_matrix_UB_32      0.0828625000
_diffrn_orient_matrix_UB_33      -0.0101645000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52298
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         66.347
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.450
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       cube
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 4318 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     702
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+2.0678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                10029
_reflns_number_total             10465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh140089_2_fa
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_original_cell_volume        5989.78(11)
_cod_database_code               7040543
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C69 H51 O4 P2 Cl5 Pd1'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C35(H35)
3.b Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3(H3), C3'(H3'), C4(H4), C4'(H4'), C5(H5), C5'(H5'), C6(H6),
 C6'(H6'), C7(H7), C7'(H7'), C8(H8), C8'(H8'), C14(H14), C14'(H14'), C15(H15),
 C15'(H15'), C16(H16), C16'(H16'), C19'(H19'), C20(H20), C20'(H20'), C21(H21),
 C21'(H21'), C22(H22), C22'(H22'), C23(H23), C23'(H23'), C24(H24), C24'(H24'),
 C25(H25), C25'(H25'), C31(H31), C31'(H31'), C32(H32), C32'(H32'), C33(H33),
 C33'(H33')
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F), C34(H34A,H34B,H34C), C34'(H34D,
 H34E,H34F)
;
_shelx_res_checksum              85084
_olex2_submission_special_instructions 'No special instructions were received'