Synthesis of Novel Terminal Iridium Phosphinidene Complexes
Termaten, Arjan T.; Nijbacker, Tom; Schakel, Marius; Lutz, Martin; Spek, Anthony L.; Lammertsma, Koop; Organometallics 21 (2002) 3196–; doi:10.1021/om020062t

data_4076805
_publ_section_title
;
 Synthesis of Novel Terminal Iridium Phosphinidene Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3196
_journal_paper_doi               10.1021/om020062t
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C46 H59 Ir P2'
_chemical_formula_sum            'C46 H59 Ir P2'
_chemical_formula_weight         866.07
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.8313(5)
_cell_angle_beta                 78.2842(5)
_cell_angle_gamma                72.4545(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7474(1)
_cell_length_b                   14.4034(2)
_cell_length_c                   16.9057(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2040.49(4)
_computing_cell_refinement       'DENZO 1.11.0'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO 1.11.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51672
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.380
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+1.3409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                8758
_reflns_number_total             9232
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om020062t.cif
_cod_data_source_block           s2276a
_cod_database_code               4076805