Unusual Pathways for Metal-Assisted C-C and C-P Coupling Reactions Using Allenylidenerhodium Complexes as Precursors
Helmut Werner; Ralf Wiedemann; Matthias Laubender; Bettina Windmüller; Paul Steinert; Olaf Gevert; Justin Wolf; Journal of the American Chemical Society 124 (2002) 6966–6980; doi:10.1021/ja012479g

data_4114866
_publ_contact_author
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        Prof. Dr. Helmut Werner
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland
        D-97074 W\"urzburg
        Deutschland
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_publ_contact_author_email       helmut.werner@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 888 4605'
_publ_contact_author_phone       '049 931 888 5261'
_publ_section_title
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 Unusual Pathways for Metal-Assisted C-C and C-P Coupling Reactions Using
 Allenylidenerhodium Complexes as Precursors
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6966
_journal_page_last               6980
_journal_paper_doi               10.1021/ja012479g
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C33.5 H52 Cl4 P2 Rh'
_chemical_formula_weight         761.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.00(3)
_cell_angle_beta                 97.90(2)
_cell_angle_gamma                108.25(2)
_cell_formula_units_Z            2
_cell_length_a                   9.463(4)
_cell_length_b                   11.369(5)
_cell_length_c                   17.936(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      8
_cell_volume                     1808.9(15)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_computing_molecular_graphics    'ZORTEP (Zsolnai)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5618
_diffrn_reflns_theta_max         23.93
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_obs          0.0317
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.8768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0858
_refine_ls_wR_factor_obs         0.0791
_reflns_number_observed          4411
_reflns_number_total             5225
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja012479g_2.cif
_cod_data_source_block           ml1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.8768P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.8768P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1808.8(14)
_cod_original_formula_sum        'C33.50 H52 Cl4 P2 Rh'
_cod_database_code               4114866