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_7037443
_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         'C36 H28 Cl O2 P Pd'
_chemical_formula_sum            'C36 H28 Cl O2 P Pd'
_chemical_formula_weight         665.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-19
_audit_creation_method
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Olex2 1.2-alpha
(compiled 2014.09.18 svn.r3010 for OlexSys, GUI svn.r4889)
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_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0618(3)
_cell_length_b                   14.4757(4)
_cell_length_c                   25.0065(10)
_cell_measurement_reflns_used    5982
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.5543
_cell_measurement_theta_min      2.9239
_cell_volume                     3642.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
  1 omega  -44.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  -77.0000 -180.0000 84

  2 omega  -44.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  -77.0000  -90.0000 83

  3 omega  -43.00  -14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  134.0000  141.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0046517000
_diffrn_orient_matrix_UB_12      -0.0465054000
_diffrn_orient_matrix_UB_13      0.0087435000
_diffrn_orient_matrix_UB_21      -0.0013921000
_diffrn_orient_matrix_UB_22      0.0151053000
_diffrn_orient_matrix_UB_23      0.0269623000
_diffrn_orient_matrix_UB_31      -0.0703575000
_diffrn_orient_matrix_UB_32      -0.0034188000
_diffrn_orient_matrix_UB_33      0.0000522000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7676
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.617
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 2545 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0376P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.687
_reflns_friedel_fraction_full    0.956
_reflns_friedel_fraction_max     0.752
_reflns_number_gt                6717
_reflns_number_total             7674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04475h2.cif
_cod_data_source_block           ljh184
_cod_depositor_comments
'Adding full bibliography for 7037441--7037444.cif.'
_cod_database_code               7037443
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C36 H28 Cl O2 P Pd'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.780
_reflns_odcompleteness_completeness 99.62
_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 Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
2.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'), C13(H13), C13'(H13'), C14(H14),
 C14'(H14'), C15(H15), C15'(H15'), C16(H16), C16'(H16')
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              78366
_olex2_submission_special_instructions 'No special instructions were received'