Chemistry of M(allyl)3 (M = Rh, Ir) compounds: structural characterization of tris(allyl)iridium complexes with phosphorus ligands
John, Kevin D.; Scott, Brian L.; Baker, R. Thomas; Sattelberger, Alfred P.; Salazar, Kenneth V.; Chemical Communications  (2000) 581–; doi:10.1039/a910164k

data_7110831
_publ_contact_author
;
R. Thomas Baker
CST-18
MS J514
Los Alamos National Laboratory
Los Alamos, NM 87545 USA
;
_publ_section_title
;
 Chemistry of M(allyl)3 (M = Rh, Ir) compounds: structural
 characterization of tris(allyl)iridium complexes with phosphorus ligands
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              581
_journal_paper_doi               10.1039/a910164k
_journal_year                    2000
_chemical_formula_sum            'C53 H55 Ir P2'
_chemical_formula_weight         946.17
_chemical_name_common
;
(1,2-bis(diphenylphosphino)benzene)bis(sigma-allyl)(pi-allyl)iridium
;
_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
_cell_angle_alpha                86.058(1)
_cell_angle_beta                 71.302(1)
_cell_angle_gamma                83.341(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7816(5)
_cell_length_b                   13.5959(6)
_cell_length_c                   13.9441(6)
_cell_measurement_temperature    203(2)
_cell_volume                     1921.98(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10344
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    3.60
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multifaceted block'
_exptl_crystal_F_000             960
_exptl_crystal_preparation       'crystallized from toluene'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0421
_reflns_number_gt                6790
_reflns_number_total             7345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a910164ksup1.cif
_cod_data_source_block           ccd163a
_cod_original_formula_sum        'C39 H39 Ir P2 2(C7 H8)'
_cod_database_code               7110831