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_7040542
_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 rmad
_chemical_formula_moiety         'C68 H50 Cl2 O4 P2 Pd, 3(C H Cl3)'
_chemical_formula_sum            'C71 H53 Cl11 O4 P2 Pd'
_chemical_formula_weight         1528.42
_chemical_name_systematic
;
 ?
;
_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             2014-07-18
_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                 111.477(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5925(9)
_cell_length_b                   21.8177(11)
_cell_length_c                   14.4054(11)
_cell_measurement_reflns_used    17254
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.3340
_cell_measurement_theta_min      3.1620
_cell_volume                     3390.5(4)
_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      150.00(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details
;
  1 omega    6.00   32.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   38.0000   60.0000 26

  2 omega  -20.00   13.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -38.0000   90.0000 33

  3 omega  -64.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000  -90.0000 99

  4 omega    7.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000   90.0000 39

  5 omega   12.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000   90.0000 58

  6 omega   -8.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000   30.0000 82

  7 omega  -15.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -90.0000 -163.2525 64

  8 omega  -85.00   18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -38.0000 -150.0000 103

  9 omega  -35.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   38.0000 -150.0000 59

 10 omega   -4.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000    0.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0357370000
_diffrn_orient_matrix_UB_12      -0.0079985000
_diffrn_orient_matrix_UB_13      -0.0500381000
_diffrn_orient_matrix_UB_21      0.0551152000
_diffrn_orient_matrix_UB_22      -0.0073350000
_diffrn_orient_matrix_UB_23      -0.0082919000
_diffrn_orient_matrix_UB_31      -0.0038474000
_diffrn_orient_matrix_UB_32      -0.0306558000
_diffrn_orient_matrix_UB_33      0.0150270000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22655
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.896
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.849
_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    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 4219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.052(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13225
_refine_ls_number_restraints     787
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0212P)^2^+2.7009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.865
_reflns_Friedel_fraction_max     0.641
_reflns_number_gt                11252
_reflns_number_total             13225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh140089_fa
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_original_cell_volume        3390.4(4)
_cod_database_code               7040542
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C71 H53 O4 P2 Cl11 Pd1'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl8) = Uanis(Cl11)
Uanis(Cl10) = Uanis(Cl7)
Uanis(C36) = Uanis(C37)
Uanis(Cl6) = Uanis(Cl9)
Uanis(Cl15) = Uanis(Cl12)
Uanis(Cl13) = Uanis(Cl16)
Uanis(C38) = Uanis(C39)
Uanis(Cl14) = Uanis(Cl17)
3. 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
4. Same fragment restrains
{Cl9, Cl10, Cl11, C37}
as
{Cl6, Cl7, Cl8, C36}
{Cl15, Cl16, Cl17, C39}
as
{Cl12, Cl13, Cl14, C38}
5. Others
 Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=Sof(C37)=Sof(H37)=Sof(Cl15)=Sof(Cl16)=Sof(Cl17)=
 Sof(C39)=Sof(H39)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl7)=Sof(Cl8)=Sof(C36)=Sof(H36)=Sof(Cl12)=Sof(Cl13)=Sof(Cl14)=
 Sof(C38)=Sof(H38)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
6.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')
6.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              71427
_olex2_submission_special_instructions 'No special instructions were received'