Helical Triskelion Monophosphites as Ligands in Asymmetric Catalysis
Manfred T. Reetz; Hongchao Guo; Jun-An Ma; Richard Goddard; Richard J. Mynott; Journal of the American Chemical Society 131 (2009) 4136–4142; doi:10.1021/ja809297a

data_4104068
_publ_section_title
;
 Helical Triskelion Monophosphites as Ligands in Asymmetric Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4136
_journal_page_last               4142
_journal_paper_doi               10.1021/ja809297a
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        dichloromethane/pentane
_chemical_formula_moiety         'C69 H69 O10 P, 3(C H2 Cl2)'
_chemical_formula_sum            'C72 H75 Cl6 O10 P'
_chemical_formula_weight         1343.99
_chemical_name_systematic
; 
 tris[2'-(1-adamantylcarbonyl)oxy-1,1'-biphenyl-2-yl]phosphite oxide
 tris-dichloromethane solute
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                GUO-GB-322-01
_audit_creation_date             2007-07-12
_cell_angle_alpha                100.216(2)
_cell_angle_beta                 102.279(2)
_cell_angle_gamma                102.329(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2620(7)
_cell_length_b                   13.9991(6)
_cell_length_c                   18.9895(8)
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    100
_cell_measurement_theta_max      54.43
_cell_measurement_theta_min      2.45
_cell_volume                     3272.5(3)
_computing_cell_refinement       'PROTEUM2 (Bruker AXS, 2004)'
_computing_data_collection       'PROTEUM2 (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 30.62
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'focusing multilayer optic'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.1752
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29644
_diffrn_reflns_theta_full        64.76
_diffrn_reflns_theta_max         64.76
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.631764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker AXS (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         9886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1906
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.3124
_reflns_number_gt                4653
_reflns_number_total             9886
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja809297a_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4104068