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_7040541
_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         'C43 H39 Cl O3 P Rh'
_chemical_formula_sum            'C43 H39 Cl O3 P Rh'
_chemical_formula_weight         773.07
_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             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6504(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.69170(6)
_cell_length_b                   17.44304(12)
_cell_length_c                   20.04701(13)
_cell_measurement_reflns_used    47156
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      27.9280
_cell_measurement_theta_min      3.6360
_cell_volume                     3388.78(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1500
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -92.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -77.0000  150.0000 105

  2 omega  -53.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889   77.0000  150.0000 97

  3 omega  -89.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -57.0000 -120.0000 68

  4 omega  -44.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889   57.0000  -90.0000 96

  5 omega  -53.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889   77.0000    0.0000 108

  6 omega  -82.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -57.0000    0.0000 89

  7 omega  -87.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -57.0000  -90.0000 91

  8 omega -102.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  178.0000    0.0000 70

  9 omega  -29.00   -4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826  104.0000  154.0000 25

 10 omega  -92.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -77.0000  -30.0000 108

 11 omega -102.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  178.0000  -90.0000 70

 12 omega  -50.00   56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889   38.0000  -90.0000 106

 13 omega  -89.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889  -57.0000 -180.0000 96

 14 omega  -44.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889   57.0000   90.0000 96

 15 omega   -4.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826  -99.0000  -60.0000 70

 16 omega   -6.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826   57.0000  120.0000 96

 17 omega -100.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889 -178.0000 -180.0000 65

 18 omega -100.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5889 -178.0000 -120.0000 65

 19 omega   -4.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826  -99.0000   30.0000 70

 20 omega  -15.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826   77.0000  -60.0000 108

 21 omega   53.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826 -178.0000 -120.0000 50

 22 omega  -14.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6826   38.0000   30.0000 108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0609609000
_diffrn_orient_matrix_UB_12      -0.0208219000
_diffrn_orient_matrix_UB_13      -0.0077809000
_diffrn_orient_matrix_UB_21      -0.0231239000
_diffrn_orient_matrix_UB_22      0.0051914000
_diffrn_orient_matrix_UB_23      0.0331403000
_diffrn_orient_matrix_UB_31      -0.0332599000
_diffrn_orient_matrix_UB_32      0.0345346000
_diffrn_orient_matrix_UB_33      -0.0096679000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107785
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.617
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 6197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0429P)^2^+3.4456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                14049
_reflns_number_total             15240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh150002_fa
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_database_code               7040541
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C43 H39 O3 P1 Cl1 Rh'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C23(H23), C24(H24), C45(H45), C46(H46), C49(H49), C50(H50)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C47(H47A,
 H47B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,H52B)
2.c 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'), C29(H29), C29'(H29'), C30(H30), C30'(H30'), C31(H31),
 C31'(H31'), C32(H32), C32'(H32'), C33(H33), C33'(H33'), C34(H34), C34'(H34'),
 C40(H40), C40'(H40'), C41(H41), C41'(H41'), C42(H42), C42'(H42')
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17'(H17D,H17E,H17F), C18(H18A,H18B,H18C), C43(H43A,H43B,
 H43C), C43'(H43D,H43E,H43F), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              68124
_olex2_submission_special_instructions 'No special instructions were received'