Phenoxaphosphine-Based Diphosphine Ligands. Synthesis and Application in the Hydroformylation Reaction
Zuidema, Erik; Goudriaan, P. Elsbeth; Swennenhuis, Bert H. G.; Kamer, Paul C. J.; van Leeuwen, Piet W. N. M.; Lutz, Martin; Spek, Anthony L.; Organometallics 29 (2010) 1210–; doi:10.1021/om901041r

data_4067619
_publ_section_title
;
 Phenoxaphosphine-Based Diphosphine Ligands. Synthesis and Application in
 the Hydroformylation Reaction
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1210
_journal_paper_doi               10.1021/om901041r
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C34 H28 O2 P2'
_chemical_formula_sum            'C34 H28 O2 P2'
_chemical_formula_weight         530.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.849(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2531(18)
_cell_length_b                   7.8060(4)
_cell_length_c                   17.0051(8)
_cell_measurement_reflns_used    19716
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.64
_cell_volume                     2682.4(3)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0092
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34055
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0402P)^2^+3.1686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                2859
_reflns_number_total             3086
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om901041r_si_002.cif
_cod_data_source_block           s3434a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4067619