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_4084431
_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            'C57 H55 O11 P2 Rh'
_chemical_formula_weight         1080.86
_chemical_name_common            (L2)Rh(crotyl)(CO)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.162(2)
_cell_length_b                   22.034(3)
_cell_length_c                   30.430(4)
_cell_measurement_reflns_used    7780
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.19
_cell_measurement_theta_min      2.28
_cell_volume                     10166(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            104189
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9258
_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    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         12657
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+18.0852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                9994
_reflns_number_total             12657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500643t_si_002.cif
_cod_data_source_block           ses3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084429--4084431.cif.
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4084431