Iridium Phosphinidene Complexes: A Comparison with Iridium Imido Complexes in Their Reaction with Isocyanides
Halil Aktas; Jos Mulder; Frans J. J. de Kanter; J. Chris Slootweg; Marius Schakel; Andreas W. Ehlers; Martin Lutz; Anthony L. Spek; Koop Lammertsma; Journal of the American Chemical Society 131 (2009) 13531–13537; doi:10.1021/ja9048509

data_4105028
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Iridium Phosphinidene Complexes: A Comparison with Iridium Imido
 Complexes in Their Reaction with Isocyanides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13531
_journal_page_last               13537
_journal_paper_doi               10.1021/ja9048509
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C46 H62 Ir N2 P'
_chemical_formula_sum            'C46 H62 Ir N2 P'
_chemical_formula_weight         866.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.067(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3239(4)
_cell_length_b                   16.0921(4)
_cell_length_c                   21.5079(7)
_cell_measurement_reflns_used    28899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.69
_cell_volume                     4201.2(2)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69676
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+2.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0391
_reflns_number_gt                7990
_reflns_number_total             9645
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9048509_si_002_2.cif
_cod_data_source_block           s3790a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105028