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_7040544
_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         'C70 H54 Cl2 O6 P2 Pd'
_chemical_formula_sum            'C70 H54 Cl2 O6 P2 Pd'
_chemical_formula_weight         1230.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7126(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.28960(10)
_cell_length_b                   20.94262(17)
_cell_length_c                   14.09792(13)
_cell_measurement_reflns_used    20338
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7970
_cell_measurement_theta_min      3.1860
_cell_volume                     3263.82(5)
_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, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -80.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  125.0000  -90.0000 62

  2 omega  -84.00  -57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  125.0000  -60.0000 27

  3 omega  -88.00  -62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  -38.0000   30.0000 26

  4 omega   17.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000  150.0000 98

  5 omega   -3.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -125.0000 -120.0000 99

  6 omega   51.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000   60.0000 65

  7 omega   60.00  102.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   60.0000 42

  8 omega  133.00  160.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 27

  9 omega  120.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 27

 10 omega   62.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 89

 11 omega   64.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -90.0000 67

 12 omega   82.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000 -112.7680 46

 13 omega   69.00  127.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -150.0000 58

 14 omega   77.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -90.0000 63

 15 omega   19.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 54

 16 omega  118.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -30.0000 27

 17 omega  117.00  154.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -90.0000 37

 18 omega   17.00   92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -90.0000 75

 19 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 26

 20 omega   63.00  164.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 101

 21 omega   19.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -180.0000 64

 22 omega    9.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -120.0000 54

 23 omega   54.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   30.0000 59

 24 omega   12.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000 -112.7680 63

 25 omega   21.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 49

 26 omega   22.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -120.0000 28

 27 omega   78.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 37

 28 omega   36.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 34

 29 omega   69.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 78

 30 omega   84.00  110.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000    0.0000 26

 31 omega  145.00  172.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -90.0000 27

 32 omega   16.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 42

 33 omega  143.00  168.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 25

 34 omega   36.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 25

 35 omega   40.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 36

 36 omega   62.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 27

 37 omega   66.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   60.0000 47

 38 omega   41.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 25

 39 omega -120.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  -77.0000  -30.0000 112

 40 omega  -99.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  125.0000    0.0000 81

 41 omega -116.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  -57.0000   30.0000 37
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1337132000
_diffrn_orient_matrix_UB_12      0.0135230000
_diffrn_orient_matrix_UB_13      -0.0018387000
_diffrn_orient_matrix_UB_21      -0.0395493000
_diffrn_orient_matrix_UB_22      0.0450405000
_diffrn_orient_matrix_UB_23      -0.0871045000
_diffrn_orient_matrix_UB_31      -0.0004804000
_diffrn_orient_matrix_UB_32      0.0565217000
_diffrn_orient_matrix_UB_33      0.0697383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.919
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.897
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.424
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 4858 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         11588
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.4386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                10738
_reflns_number_total             11588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh150009_fa
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_database_code               7040544
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C72 H58 O6 P2 Cl6 Pd1'
_reflns_odcompleteness_completeness 99.92
_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.a Aromatic/amide H refined with riding coordinates:
 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'), C21(H21), C21'(H21'), C22(H22), C22'(H22'), C23(H23),
 C23'(H23'), C24(H24), C24'(H24'), C25(H25), C25'(H25'), C26(H26), C26'(H26'),
 C32(H32), C32'(H32'), C33(H33), C33'(H33'), C34(H34), C34'(H34')
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F), C18(H18A,H18B,H18C), C35(H35A,H35B,
 H35C), C35'(H35D,H35E,H35F), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              70375
_olex2_submission_special_instructions 'No special instructions were received'