Hydrolysis Stability of Bidentate Phosphites Utilized as Modifying Ligands in the Rh-Catalyzedn-Regioselective Hydroformylation of Olefins
Zhang, Baoxin; Jiao, Haijun; Michalik, Dirk; Kloß, Svenja; Deter, Lisa Marie; Selent, Detlef; Spannenberg, Anke; Franke, Robert; Börner, Armin; ACS Catalysis 6 (2016) 7554–; doi:10.1021/acscatal.6b02185

data_4516701
_publ_section_title
;
 Hydrolysis Stability of Bidentate Phosphites Utilized as Modifying
 Ligands in the Rh-Catalyzedn-Regioselective Hydroformylation of Olefins
;
_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              7554
_journal_paper_doi               10.1021/acscatal.6b02185
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C26 H35 O5 P'
_chemical_formula_weight         458.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.4269(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4338(3)
_cell_length_b                   11.4458(3)
_cell_length_c                   23.1231(7)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.51
_cell_volume                     2475.83(13)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.505
_exptl_crystal_size_min          0.472
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0530P)^2^+0.7660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5408
_reflns_number_total             5980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b02185_si_005.cif
_cod_data_source_block           AX0965
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4516701
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97110
_shelx_hkl_checksum              49565