Reaction of Secondary Phosphine Oxides with Rhodium(I)
Christiansen, Andrea; Selent, Detlef; Spannenberg, Anke; Baumann, Wolfgang; Franke, Robert; Börner, Armin; Organometallics 29 (2010) 3139–; doi:10.1021/om100171p

data_4065863
_publ_section_title
;
 Reaction of Secondary Phosphine Oxides with Rhodium(I)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3139
_journal_paper_doi               10.1021/om100171p
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C31.5 H17 F16 N4 O2 P2 Rh'
_chemical_formula_weight         952.34
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.310(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8014(5)
_cell_length_b                   15.8180(7)
_cell_length_c                   15.8529(6)
_cell_measurement_reflns_used    41214
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      1.72
_cell_volume                     3460.8(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (J. Appl. Cryst. 2005, 38, 381)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43042
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9197
_exptl_absorpt_correction_T_min  0.5465
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                4976
_reflns_number_total             6096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100171p_si_001.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C31.50 H17 F16 N4 O2 P2 Rh'
_cod_database_code               4065863