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_7110829
_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            'C54 H60 Ir2 P2'
_chemical_formula_weight         1155.36
_chemical_name_common
;
(triphenylphosphine)(sigma-allyl)bis(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                73.249(1)
_cell_angle_beta                 82.344(1)
_cell_angle_gamma                79.303(1)
_cell_formula_units_Z            4
_cell_length_a                   9.2972(4)
_cell_length_b                   15.7287(7)
_cell_length_c                   16.6995(8)
_cell_measurement_temperature    203(2)
_cell_volume                     2289.49(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8678
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    11.824
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multifaceted block'
_exptl_crystal_F_000             2272
_exptl_crystal_preparation       'crystallized from toluene'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.940
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                7576
_reflns_number_total             8678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a910164ksup1.cif
_cod_data_source_block           ccd130
_cod_database_code               7110829