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_7040538
_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         'C40 H33 Cl O2 P Rh'
_chemical_formula_sum            'C40 H33 Cl O2 P Rh'
_chemical_formula_weight         714.99
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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            6
_cell_length_a                   10.4774(2)
_cell_length_b                   10.4774(2)
_cell_length_c                   49.1495(16)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.1470
_cell_measurement_theta_min      2.7849
_cell_volume                     4672.6(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
  1 omega  -90.00   18.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.5696  -38.0000   90.0000 144

  2 omega -102.00  -54.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.5696  179.0000   30.0000 64

  3 omega  -34.00   -7.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2102  110.0000  157.0000 36

  4 omega   -1.00   26.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2102  -99.0000  -60.0000 36

  5 omega    7.00   82.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2102   57.0000  -30.0000 100

  6 omega   58.00   83.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2102  179.0000   60.0000 34
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0265880000
_diffrn_orient_matrix_UB_12      0.0004194000
_diffrn_orient_matrix_UB_13      -0.0132458000
_diffrn_orient_matrix_UB_21      -0.0161472000
_diffrn_orient_matrix_UB_22      0.0553102000
_diffrn_orient_matrix_UB_23      0.0041099000
_diffrn_orient_matrix_UB_31      0.0717253000
_diffrn_orient_matrix_UB_32      0.0552072000
_diffrn_orient_matrix_UB_33      -0.0039849000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            31490
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.209
_diffrn_reflns_theta_min         2.791
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76010
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.661
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 2919 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0574
_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^)+18.9687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.831
_reflns_number_gt                6646
_reflns_number_total             6807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02390h2.cif
_cod_data_source_block           ljh130003
_cod_depositor_comments
;Adding full bibliography for 7040537--7040545.cif.

 Adding full bibliography for 7040537--7040545.cif.
;
_cod_database_code               7040538
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.65
_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
2.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C21(H21), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B)
2.c 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'), C13(H13), C13'(H13'), C14(H14),
 C14'(H14'), C15(H15), C15'(H15'), C16(H16), C16'(H16')
;
_shelx_res_checksum              72243
_olex2_submission_special_instructions 'No special instructions were received'