The design of second generation MOP-phosphonites: efficient chiral hydrosilylation of functionalised styrenes.
Fleming, James T.; Ficks, Arne; Waddell, Paul G.; Harrington, Ross W.; Higham, Lee J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1886–1890; doi:10.1039/c5dt04475h

data_7037444
_publ_section_title
;
 The design of second generation MOP-phosphonites: efficient chiral
 hydrosilylation of functionalised styrenes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1886
_journal_page_last               1890
_journal_paper_doi               10.1039/c5dt04475h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H32 Cl O2 P Pd'
_chemical_formula_sum            'C38 H32 Cl O2 P Pd'
_chemical_formula_weight         693.45
_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             2014-06-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.05.21 svn.r2942 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-08-02 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6112(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4401(2)
_cell_length_b                   16.7063(3)
_cell_length_c                   16.3663(3)
_cell_measurement_reflns_used    28040
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.0470
_cell_measurement_theta_min      3.2790
_cell_volume                     3127.78(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 0.998
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
  1 omega  -25.00   33.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   92.0000   64.0000 58

  2 omega  -16.00   86.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000    0.0000 102

  3 omega  -31.00   89.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   19.0000  -90.0000 120

  4 omega  -16.00   79.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000  120.0000 95

  5 omega  -45.00   44.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -68.0000  -62.9450 89

  6 omega  -13.00   51.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -91.0000  171.5865 64

  7 omega    8.00   61.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -111.0000 -140.0391 53

  8 omega   -1.00   57.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -104.0000   78.4715 58

  9 omega  -85.00   18.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -38.0000 -180.0000 103

 10 omega  -68.00   44.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -77.0000  -90.0000 112

 11 omega  -65.00   37.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000  120.0000 102

 12 omega  -65.00   37.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000  -60.0000 102

 13 omega    0.00   55.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       10.4695 -103.0000   92.3929 55

 14 omega    7.00   61.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -111.0000 -140.0391 54
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0249891000
_diffrn_orient_matrix_UB_12      0.0386838000
_diffrn_orient_matrix_UB_13      0.0034000000
_diffrn_orient_matrix_UB_21      0.0042150000
_diffrn_orient_matrix_UB_22      0.0050818000
_diffrn_orient_matrix_UB_23      -0.0429099000
_diffrn_orient_matrix_UB_31      -0.0565923000
_diffrn_orient_matrix_UB_32      -0.0167031000
_diffrn_orient_matrix_UB_33      -0.0051860000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            96971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.458
_diffrn_reflns_theta_min         2.772
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.871
_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    1.473
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 5230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.056(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         15384
_refine_ls_number_restraints     826
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0245P)^2^+1.5381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.856
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.845
_reflns_number_gt                12583
_reflns_number_total             15384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04475h2.cif
_cod_data_source_block           ljh130062_off_fa
_cod_depositor_comments
'Adding full bibliography for 7037441--7037444.cif.'
_cod_database_code               7037444
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C38 H32 O2 P1 Cl1 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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C42A) = Uanis(C42B)
Uanis(C40A) = Uanis(C40B)
Uanis(C41A) = Uanis(C41B)
Uanis(Pd2A) = Uanis(Pd2B)
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. Others
 Sof(Pd2B)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=
 Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(Pd2A)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=
 Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C40A(H40A,H40B), C40B(H40C,H40D), C41A(H41A,
 H41B), C41B(H41C,H41D)
5.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'), C23'(H23'), C24(H24), C24'(H24'), C25(H25),
 C25'(H25'), C26(H26), C26'(H26'), C27(H27), C27'(H27'), C28(H28), C28'(H28'),
 C29(H29), C29'(H29'), C35(H35), C35'(H35'), C36(H36), C36'(H36'), C37(H37),
 C37'(H37')
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F), C21(H21A,H21B,H21C), C38(H38A,H38B,
 H38C), C38'(H38D,H38E,H38F), C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F)
;
_shelx_res_checksum              55580
_olex2_submission_special_instructions 'No special instructions were received'