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_4516703
_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            'C48 H53 O12 P2 Rh'
_chemical_formula_weight         986.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 101.7803(7)
_cell_angle_gamma                100.5595(6)
_cell_formula_units_Z            2
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_cell_length_c                   15.5406(4)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.59
_cell_volume                     2367.22(11)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
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_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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
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_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48509
_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         28.000
_diffrn_reflns_theta_min         1.701
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.268
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         11429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.5491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10387
_reflns_number_total             11429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b02185_si_003.cif
_cod_data_source_block           AX0846
_cod_database_code               4516703
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              29500
_shelx_hkl_checksum              88044