Synthesis and structures of the homoleptic cations [M(PMe3)5]+ (M = Rh, Ir)
Rivers, Joseph H.; Jones, Richard A.; Chemical Communications 46 (2010) 4300–4302; doi:10.1039/c0cc00892c

data_7111758
_publ_section_title
;
 Synthesis and structures of the homoleptic cations [M(PMe3)5]+ (M = Rh,
 Ir)
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              4300
_journal_page_last               4302
_journal_paper_doi               10.1039/c0cc00892c
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C15 H45 P5 Rh, C5 H F6 N2'
_chemical_formula_sum            'C20 H46 F6 N2 P5 Rh'
_chemical_formula_weight         686.35
_chemical_name_common
;pentakis(trimethylphosphine)rhodium(i) bis(3,5-
trifluoromethyl)pyrazolate
;
_chemical_name_systematic
;
pentakis(trimethylphosphine)rhodium(I) bis(3,5-trifluoromethyl)pyrazolate
;
_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
_cell_angle_alpha                88.422(4)
_cell_angle_beta                 75.798(3)
_cell_angle_gamma                77.305(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4967(11)
_cell_length_b                   12.0818(14)
_cell_length_c                   14.6363(17)
_cell_measurement_reflns_used    22713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.92
_cell_measurement_theta_min      6.28
_cell_volume                     1587.6(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27263
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001).
The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.802
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+2.2373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                6910
_reflns_number_total             7227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc00892csup1.cif
_cod_data_source_block           RhP5Pz
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111758