Perfluoroalkylation of Coordinated Ethene in Rh(I) and Ir(I) Complexes. Catalytic Addition of Iodoperfluoroalkanes to Ethene
Blaya, María; Bautista, Delia; Gil-Rubio, Juan; Vicente, José; Organometallics 36 (2017) 1245–; doi:10.1021/acs.organomet.6b00929

data_4087292
_publ_section_title
;
 Perfluoroalkylation of Coordinated Ethene in Rh(I) and Ir(I) Complexes.
 Catalytic Addition of Iodoperfluoroalkanes to Ethene
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1245
_journal_paper_doi               10.1021/acs.organomet.6b00929
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C47 H44 F3 Ir O3 P2 S'
_chemical_formula_weight         1000.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5419(12)
_cell_length_b                   12.8656(11)
_cell_length_c                   20.1928(16)
_cell_measurement_reflns_used    6821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.29
_cell_volume                     4037.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruke SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25467
_diffrn_reflns_point_group_measured_fraction_full 0.876
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.680
_diffrn_reflns_theta_min         1.877
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  0.6792
_exptl_absorpt_correction_T_min  0.4929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.229
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 2808 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8219
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.635
_reflns_Friedel_fraction_full    0.743
_reflns_Friedel_fraction_max     0.629
_reflns_number_gt                7741
_reflns_number_total             8219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00929_si_002.cif
_cod_data_source_block           mbm1642sib
_cod_database_code               4087292
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.343
_shelx_estimated_absorpt_t_max   0.679
_shelx_res_checksum              65330
_shelx_hkl_checksum              38969