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_7040537
_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         'C39 H38 Cl2 O3 P2 Pt'
_chemical_formula_sum            'C39 H38 Cl2 O3 P2 Pt'
_chemical_formula_weight         882.62
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.05.21 svn.r2942 for OlexSys, GUI svn.r4846)
;
_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                120
_cell_formula_units_Z            3
_cell_length_a                   11.52064(15)
_cell_length_b                   11.52064(15)
_cell_length_c                   22.9152(3)
_cell_measurement_reflns_used    36291
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.2840
_cell_measurement_theta_min      3.3130
_cell_volume                     2633.95(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega  -67.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209  -77.0000   90.0000 93

  2 omega -110.00  -35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209 -179.0000   30.0000 75

  3 omega  -22.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053   57.0000   30.0000 94

  4 omega  -42.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053   19.0000  -30.0000 118

  5 omega  -68.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053  -57.0000    0.0000 118

  6 omega  -65.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053  -57.0000 -120.0000 117

  7 omega   55.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053 -131.0000  -32.7014 26

  8 omega -109.00  -32.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209  179.0000 -150.0000 77

  9 omega  -50.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209   57.0000 -120.0000 121

 10 omega  -50.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209   57.0000   30.0000 121

 11 omega -105.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209  -77.0000  -60.0000 131

 12 omega  -98.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5209  -57.0000   90.0000 121

 13 omega  -81.00  -34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053 -179.0000   60.0000 47

 14 omega  -22.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053   57.0000   30.0000 121

 15 omega   22.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053 -131.0000  -32.7014 59

 16 omega   -4.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0053  -99.0000  120.0000 66
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0639308000
_diffrn_orient_matrix_UB_12      -0.0391761000
_diffrn_orient_matrix_UB_13      -0.0130312000
_diffrn_orient_matrix_UB_21      0.0173682000
_diffrn_orient_matrix_UB_22      0.0495762000
_diffrn_orient_matrix_UB_23      -0.0218819000
_diffrn_orient_matrix_UB_31      0.0257709000
_diffrn_orient_matrix_UB_32      -0.0325661000
_diffrn_orient_matrix_UB_33      -0.0176021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83576
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.398
_diffrn_reflns_theta_min         2.707
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.276
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.538
_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    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 3745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0247(18)
_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     428
_refine_ls_number_reflns         8250
_refine_ls_number_restraints     400
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0129P)^2^+1.2122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0363
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                7956
_reflns_number_total             8250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh130058_4_fa
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_original_cell_volume        2633.95(8)
_cod_database_code               7040537
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C39 H38 O3 Cl2 P2 Pt1'
_reflns_odcompleteness_completeness 99.81
_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. 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 Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B)
3.b 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'), C13(H13), C13'(H13'), C14(H14), C14'(H14'),
  C15(H15), C15'(H15'), C16(H16), C16'(H16')
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              95601
_olex2_submission_special_instructions 'No special instructions were received'