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_7040539
_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         'C41 H35 Cl O3 P Rh'
_chemical_formula_sum            'C41 H35 Cl O3 P Rh'
_chemical_formula_weight         745.02
_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             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
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.6324(3)
_cell_length_b                   10.6324(3)
_cell_length_c                   24.9502(8)
_cell_measurement_reflns_used    6208
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3626
_cell_measurement_theta_min      3.2594
_cell_volume                     2442.68(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details
;
  1 omega   -1.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257  -99.0000 -150.0000 44

  2 omega   -6.00   20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257   89.0000 -168.0000 26

  3 omega   -4.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257  -99.0000  -60.0000 56

  4 omega  -39.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257  -57.0000    0.0000 78

  5 omega  -17.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257   38.0000  -30.0000 40
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0112273000
_diffrn_orient_matrix_UB_12      0.0477909000
_diffrn_orient_matrix_UB_13      0.0165169000
_diffrn_orient_matrix_UB_21      0.0755479000
_diffrn_orient_matrix_UB_22      0.0507145000
_diffrn_orient_matrix_UB_23      -0.0006073000
_diffrn_orient_matrix_UB_31      -0.0099746000
_diffrn_orient_matrix_UB_32      0.0328120000
_diffrn_orient_matrix_UB_33      -0.0231412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15538
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 2701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.059(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.768
_reflns_number_gt                6255
_reflns_number_total             6762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh130002
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_original_cell_volume        2442.68(16)
_cod_database_code               7040539
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C41 H35 Cl O3 P Rh'
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.851
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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:
 C18(H18), C19(H19), C22(H22), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B)
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'), C13(H13), C13'(H13'), C14(H14), C14'(H14'),
  C15(H15), C15'(H15'), C16(H16), C16'(H16')
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              15568
_olex2_submission_special_instructions 'No special instructions were received'