Rhodium(I) Silyl Complexes for C‒F Bond Activation Reactions of Aromatic Compounds: Experimental and Computational Studies
Raza, Anna Lena; Panetier, Julien A.; Teltewskoi, Michael; Macgregor, Stuart A.; Braun, Thomas; Organometallics 32 (2013) 3795–; doi:10.1021/om400150p

data_4080925
_publ_section_title
;
 Rhodium(I) Silyl Complexes for C--F Bond Activation Reactions of Aromatic
 Compounds: Experimental and Computational Studies
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3795
_journal_paper_doi               10.1021/om400150p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C24 H45 F5 P3 Rh'
_chemical_formula_sum            'C24 H45 F5 P3 Rh'
_chemical_formula_weight         624.42
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.021(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3377(3)
_cell_length_b                   18.0790(4)
_cell_length_c                   16.7460(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      1.94
_cell_volume                     2826.55(14)
_computing_cell_refinement       'X-AREA (Stoe &amp; Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe &amp; Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe &amp; Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg &amp; Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,220 exposures'
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30069
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.8802
_exptl_absorpt_correction_T_min  0.7572
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After 
that a numerical absorption correction basing on a Gaussian algorithsm 
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0024(2)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         7512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.6684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                6964
_reflns_number_total             7512
_reflns_threshold_expression     I&gt;2sigma(I)
_cod_data_source_file            om400150p_si_002.cif
_cod_data_source_block           c:\anna\micha14
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4080925