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_7037442
_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         'C33 H23 O3 P'
_chemical_formula_sum            'C33 H23 O3 P'
_chemical_formula_weight         498.48
_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             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                 107.242(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5367(15)
_cell_length_b                   14.1786(15)
_cell_length_c                   9.6102(11)
_cell_measurement_reflns_used    885
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.5000
_cell_measurement_theta_min      2.8675
_cell_volume                     1241.1(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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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 0.955
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega    0.00   28.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  -99.0000  -30.0000 28

  2 omega    7.00   86.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038   38.0000  120.0000 79

  3 omega  -23.00   53.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038   19.0000   90.0000 76
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0648329000
_diffrn_orient_matrix_UB_12      -0.0197125000
_diffrn_orient_matrix_UB_13      0.0097613000
_diffrn_orient_matrix_UB_21      0.0399846000
_diffrn_orient_matrix_UB_22      -0.0406389000
_diffrn_orient_matrix_UB_23      0.0319536000
_diffrn_orient_matrix_UB_31      0.0162682000
_diffrn_orient_matrix_UB_32      0.0214634000
_diffrn_orient_matrix_UB_33      0.0696740000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5355
_diffrn_reflns_point_group_measured_fraction_full 0.768
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98359
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(17)
_refine_ls_extinction_coef       0.0071(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3452
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.539
_reflns_Friedel_fraction_full    0.563
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                2575
_reflns_number_total             3452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04475h2.cif
_cod_data_source_block           ljh130007
_cod_depositor_comments
'Adding full bibliography for 7037441--7037444.cif.'
_cod_database_code               7037442
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C17'(H17A,H17B,H17C)
2.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')
;
_shelx_res_checksum              6818
_olex2_submission_special_instructions 'No special instructions were received'