Competing reaction pathways of 3,3,3-trifluoropropene at rhodium hydrido, silyl and germyl complexes: C-F bond activation versus hydrogermylation.
Ahrens, Theresia; Teltewskoi, Michael; Ahrens, Mike; Braun, Thomas; Laubenstein, Reik; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17495–17507; doi:10.1039/c6dt03027k

data_7040920
_publ_section_title
;
 Competing reaction pathways of 3,3,3-trifluoropropene at rhodium hydrido,
 silyl and germyl complexes: C-F bond activation versus hydrogermylation.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17495
_journal_page_last               17507
_journal_paper_doi               10.1039/c6dt03027k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C21 H18 F2 Ge'
_chemical_formula_sum            'C21 H18 F2 Ge'
_chemical_formula_weight         380.94
_chemical_name_systematic        Compound_7
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                67.024(2)
_cell_angle_beta                 83.103(2)
_cell_angle_gamma                84.211(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4950(4)
_cell_length_b                   9.7733(4)
_cell_length_c                   10.3171(4)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.16
_cell_volume                     873.54(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28469
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.6105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                4079
_reflns_number_total             4346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03027k2.cif
_cod_data_source_block           Compound_7
_cod_depositor_comments
'Adding full bibliography for 7040919--7040920.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7040920