Oxidative formation of phosphinyl radicals from a trigonal pyramidal terminal phosphide Rh(i) complex, with an unusually long Rh-P bond.
Fischbach, Urs; Trincado, M.; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3443–3448; doi:10.1039/c7dt00070g

data_7041990
_publ_section_title
;
 Oxidative formation of phosphinyl radicals from a trigonal pyramidal
 terminal phosphide Rh(i) complex, with an unusually long Rh-P bond.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3443
_journal_page_last               3448
_journal_paper_doi               10.1039/c7dt00070g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C46 H33 F3 O3 P Rh S'
_chemical_formula_sum            'C46 H33 F3 O3 P Rh S'
_chemical_formula_weight         856.66
_chemical_name_common
(trifluoromethanesulfonato)[tris(trop)phosphane]rhodium(I)
_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           'form.cif (version 2.0)'
_audit_update_record
;
2017-01-06 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.4290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0718(11)
_cell_length_b                   18.2712(16)
_cell_length_c                   15.6047(13)
_cell_measurement_temperature    200(2)
_cell_volume                     3625.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Apex with CCD'
_diffrn_measurement_method       'phi and omega 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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25467
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.8946
_exptl_absorpt_correction_T_min  0.8184
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+3.4857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                4716
_reflns_number_total             6190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00070g2.cif
_cod_data_source_block           Rhtrop3POTf
_cod_depositor_comments
'Adding full bibliography for 7041989--7041991.cif.'
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7041990