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_4068466
_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 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.367(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0340(6)
_cell_length_b                   15.2010(6)
_cell_length_c                   19.6740(4)
_cell_measurement_reflns_used    6582
_cell_measurement_temperature    100.0(10)
_cell_volume                     4401.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0635267
_diffrn_orient_matrix_UB_12      -0.0070763
_diffrn_orient_matrix_UB_13      -0.0033609
_diffrn_orient_matrix_UB_21      0.0125991
_diffrn_orient_matrix_UB_22      -0.063187
_diffrn_orient_matrix_UB_23      0.0146141
_diffrn_orient_matrix_UB_31      0.0205323
_diffrn_orient_matrix_UB_32      0.0168789
_diffrn_orient_matrix_UB_33      0.0532995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0418
_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            58594
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.467
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+31.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.175
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                6486
_reflns_number_total             8048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800867h_si_001.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068466