Iridium(I) Complexes of Upper Rim Functionalized PTA Derivatives. Synthesis, Characterization, and Use in Catalytic Hydrogenations (PTA = 1,3,5-Triaaza-7-phosphaadamantane)
Guerriero, Antonella; Erlandsson, Mikael; Ienco, Andrea; Krogstad, Donald A.; Peruzzini, Maurizio; Reginato, Gianna; Gonsalvi, Luca; Organometallics 30 (2011) 1874–; doi:10.1021/om1011177

data_4064082
_publ_section_title
;
 Iridium(I) Complexes of Upper Rim Functionalized PTA Derivatives.
 Synthesis, Characterization, and Use in Catalytic Hydrogenations (PTA =
 1,3,5-Triaaza-7-phosphaadamantane)
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1874
_journal_paper_doi               10.1021/om1011177
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H23 N4 O1 P1'
_chemical_formula_sum            'C15 H23 N4 O P'
_chemical_formula_weight         306.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2008-10-25T12:48:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.984(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5675(19)
_cell_length_b                   7.7963(8)
_cell_length_c                   12.4241(16)
_cell_measurement_reflns_used    3726
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.2136
_cell_measurement_theta_min      3.8731
_cell_measurement_wavelength     0.71073
_cell_volume                     1517.5(3)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.904
_diffrn_orient_matrix_UB_11      -0.0543954673
_diffrn_orient_matrix_UB_12      0.018230838
_diffrn_orient_matrix_UB_13      0.0035300786
_diffrn_orient_matrix_UB_21      0.0202439915
_diffrn_orient_matrix_UB_22      -0.02378509
_diffrn_orient_matrix_UB_23      0.0435693373
_diffrn_orient_matrix_UB_31      0.0168615461
_diffrn_orient_matrix_UB_32      0.0858685774
_diffrn_orient_matrix_UB_33      0.0113337865
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11990
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         32.36
_diffrn_reflns_theta_min         3.9
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                2845
_reflns_number_total             4915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011177_si_002.cif
_cod_data_source_block           pant64a
_cod_database_code               4064082