Facile Single or Double C−H Bond Activation on a Cp* Ligand Promoted by the Presence of Alkynylphosphine Ligands
Bernechea, María; Berenguer, Jesús R.; Lalinde, Elena; Torroba, Javier; Organometallics 28 (2009) 312–; doi:10.1021/om800867h

data_4068465
_publ_section_title
;
 Facile Single or Double C&#x2212;H Bond Activation on a Cp* Ligand
 Promoted by the Presence of Alkynylphosphine Ligands
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              312
_journal_paper_doi               10.1021/om800867h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C51 H45 Cl F3 O3 P2 Rh S'
_chemical_formula_weight         995.23
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.5170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4650(3)
_cell_length_b                   15.0860(3)
_cell_length_c                   19.0140(4)
_cell_measurement_reflns_used    45712
_cell_measurement_temperature    123.0(10)
_cell_volume                     4435.88(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0191309
_diffrn_orient_matrix_UB_12      0.0592128
_diffrn_orient_matrix_UB_13      -0.0179375
_diffrn_orient_matrix_UB_21      0.0442007
_diffrn_orient_matrix_UB_22      0.0295257
_diffrn_orient_matrix_UB_23      0.0307371
_diffrn_orient_matrix_UB_31      0.0431509
_diffrn_orient_matrix_UB_32      -0.003992
_diffrn_orient_matrix_UB_33      -0.0387261
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32930
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.565
_refine_diff_density_min         -2.07
_refine_diff_density_rms         0.28
_refine_ls_extinction_coef       0.0126(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9033
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          3.643
_refine_ls_shift/su_mean         0.059
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1724P)^2^+13.6069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2644
_reflns_number_gt                6883
_reflns_number_total             9033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800867h_si_001.cif
_cod_data_source_block           1,2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4068465