Rhodium and iridium complexes with 2-(diphenylphosphanyl)anilido ligands: reactions with phenylacetylene and dimethyl acetylenedicarboxylate †
Dahlenburg, Lutz; Herbst, Konrad; Journal of the Chemical Society, Dalton Transactions  (1999) 3935–; doi:10.1039/a906430c

data_7027754
_publ_section_title
;
 Rhodium and iridium complexes with 2-(diphenylphosphanyl)anilido ligands:
 reactions with phenylacetylene and dimethyl
 acetylenedicarboxylate&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3935
_journal_paper_doi               10.1039/a906430c
_journal_year                    1999
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H40 Ir1 N1 O6 P2'
_chemical_formula_structural     'C44 H40 IR N O6 P2'
_chemical_formula_sum            'C44 H40 Ir N O6 P2'
_chemical_formula_weight         932.91
_chemical_name_systematic
;
 [1,2-Bis(methoxycarbonyl)vinyl-C,O-][2-(diphenylphosphanyl)phenylamido-N,P]-
 methoxycarbonyl(triphenylphosphane)iridium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1999-07-16T10:56:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.093(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3200(10)
_cell_length_b                   18.325(9)
_cell_length_c                   16.1970(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      8.1
_cell_measurement_wavelength     0.71073
_cell_volume                     3914(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8169
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
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_exptl_absorpt_correction_T_max  0.7648
_exptl_absorpt_correction_T_min  0.2416
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
 Number of psi-scan sets used was   5
 Theta correction was applied.
 Averaged transmission function was used.
 No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0734
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                4605
_reflns_number_total             6873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906430csup1.cif
_cod_data_source_block           herb09
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7027754
_diffrn_standards_decay_corr_max 1.079
_diffrn_standards_decay_corr_min 0.97