Synthesis and Characterization of Crotyl Intermediates in Rh-Catalyzed Hydroformylation of 1,3-Butadiene
Schmidt, Sebastian; Baráth, Eszter; Prommnitz, Tanja; Rosendahl, Tobias; Rominger, Frank; Hofmann, Peter; Organometallics 33 (2014) 6018–; doi:10.1021/om500643t

data_4084430
_publ_section_title
;
 Synthesis and Characterization of Crotyl Intermediates in Rh-Catalyzed
 Hydroformylation of 1,3-Butadiene
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6018
_journal_paper_doi               10.1021/om500643t
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C51 H45 Cl4 O6 P2 Rh'
_chemical_formula_weight         1060.52
_chemical_name_common            (L3)Rh(crotyl)
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                67.793(3)
_cell_angle_beta                 80.861(3)
_cell_angle_gamma                84.410(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7727(14)
_cell_length_b                   12.9970(16)
_cell_length_c                   16.418(2)
_cell_measurement_reflns_used    6726
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.28
_cell_volume                     2294.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24216
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.384
_diffrn_reflns_theta_min         1.734
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_correction_T_min  0.6287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen,             Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         11341
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+4.3237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9254
_reflns_number_total             11341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500643t_si_002.cif
_cod_data_source_block           tro25
_cod_depositor_comments
'Adding full bibliography for 4084429--4084431.cif.'
_cod_database_code               4084430
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2014-3
_shelx_res_checksum              92551