Synthesis and structure of rhodium(i) silyl carbonyl complexes: photochemical C-F and C-H bond activation of fluorinated aromatic compounds.
Zámostná, Lada; Sander, Stefan; Braun, Thomas; Laubenstein, Reik; Braun, Beatrice; Herrmann, Roy; Kläring, Paul; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9450–9469; doi:10.1039/c5dt00819k

data_7034877
_publ_section_title
;
 Synthesis and structure of rhodium(i) silyl carbonyl complexes:
 photochemical C-F and C-H bond activation of fluorinated aromatic
 compounds.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9450
_journal_page_last               9469
_journal_paper_doi               10.1039/c5dt00819k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C32 H70 O2 P4 Rh2'
_chemical_formula_sum            'C16 H35 O P2 Rh'
_chemical_formula_weight         408.29
_chemical_name_systematic
; 
 ? 
;
_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
;
2015-02-17 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.3930(19)
_cell_angle_beta                 95.2970(18)
_cell_angle_gamma                90.2790(19)
_cell_formula_units_Z            4
_cell_length_a                   7.5908(4)
_cell_length_b                   14.1700(7)
_cell_length_c                   18.0805(8)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.86
_cell_measurement_theta_min      2.69
_cell_volume                     1932.96(16)
_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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            177204
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         44.31
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.7487
_exptl_absorpt_correction_T_min  0.6524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.271
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         30661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.1171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                23469
_reflns_number_total             30661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00819k2.cif
_cod_data_source_block           complex4_lzss4c
_cod_depositor_comments
'Adding full bibliography for 7034874--7034883.cif.'
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7034877