Functionalized phosphorus analogues of the β-diketiminato ligand systems: bis(N-arylphosphinimino)acetonitrile-derived complexes of rhodium and iridium
Spannhoff, Kirsten; Kehr, Gerald; Kehr, Seda; Fröhlich, Roland; Erker, Gerhard; Dalton Transactions  (2008) 3339–3344; doi:10.1039/b802032a

data_7004019
_publ_section_title
;
 Functionalized phosphorus analogues of the \b-diketiminato ligand
 systems: bis(N-arylphosphinimino)acetonitrile-derived complexes of
 rhodium and iridium
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              3339
_journal_page_last               3344
_journal_paper_doi               10.1039/b802032a
_journal_year                    2008
_chemical_formula_sum            'C53 H50 Ir N3 P2'
_chemical_formula_weight         983.10
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.446(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7081(2)
_cell_length_b                   11.3012(1)
_cell_length_c                   21.4893(2)
_cell_measurement_reflns_used    10670
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     4454.82(8)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41726
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.108
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.4092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.4542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                8671
_reflns_number_total             10575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802032a.txt
_cod_data_source_block           erk4289
_cod_original_cell_volume        4454.82(7)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7004019