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_4087295
_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            'C32 H38 F18 I2 Ir2'
_chemical_formula_weight         1402.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     Patterson
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.707(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1205(13)
_cell_length_b                   14.3933(15)
_cell_length_c                   11.6847(12)
_cell_measurement_reflns_used    5186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.25
_cell_volume                     1962.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
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_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 0.998
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22952
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.588
_diffrn_reflns_theta_min         1.745
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.457
_exptl_absorpt_correction_T_max  0.7284
_exptl_absorpt_correction_T_min  0.4576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
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_exptl_crystal_description       block
_exptl_crystal_F_000             1304
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_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.679
_refine_diff_density_min         -2.460
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4704
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.406
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0456
_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^)+28.2614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4471
_reflns_number_total             4704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00929_si_002.cif
_cod_data_source_block           mbm892si
_cod_database_code               4087295
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.311
_shelx_estimated_absorpt_t_max   0.728
_shelx_res_checksum              44568
_shelx_hkl_checksum              99679