Diastereomerically Enriched Analogues of the Water-Soluble Phosphine PTA. Synthesis of Phenyl(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]dec-6-yl)methanol (PZA) and the Sulfide PZA(S) and X-ray Crystal Structures of the Oxide PZA(O) and [Cp*IrCl2(PZA)]
Mikael Erlandsson; Luca Gonsalvi; Andrea Ienco; Maurizio Peruzzini; Inorganic Chemistry 47 (2008) 8–10; doi:10.1021/ic701795y

data_4304314
_publ_contact_author             'Ienco, Andrea'
_publ_contact_author_email       andrea.ienco@iccom.cnr.it
_publ_section_title
;
Diastereomerically Enriched Analogues of the Water-Soluble Phosphine PTA.
Synthesis of
Phenyl(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]dec-6-yl)methanol (PZA)
and the Sulfide PZA(S) and X-ray Crystal Structures of the Oxide PZA(O) and
[Cp*IrCl2(PZA)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8
_journal_page_last               10
_journal_paper_doi               10.1021/ic701795y
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H33 Cl2 Ir1 N3 O1 P1'
_chemical_formula_sum            'C23 H33 Cl2 Ir N3 O P'
_chemical_formula_weight         661.59
_chemical_name_systematic        ?
_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             2007-07-27T11:19:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.436(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.875(10)
_cell_length_b                   13.654(19)
_cell_length_c                   20.355(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.22
_cell_measurement_theta_min      6.23
_cell_measurement_wavelength     0.71073
_cell_volume                     2467(4)
_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, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo 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 CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.094355
_diffrn_orient_matrix_UB_12      -0.01369
_diffrn_orient_matrix_UB_13      -0.025527
_diffrn_orient_matrix_UB_21      -0.061465
_diffrn_orient_matrix_UB_22      0.016343
_diffrn_orient_matrix_UB_23      0.039476
_diffrn_orient_matrix_UB_31      -0.004069
_diffrn_orient_matrix_UB_32      0.070053
_diffrn_orient_matrix_UB_33      -0.014303
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3535
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        11
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.715
_exptl_absorpt_correction_T_max  0,488664
_exptl_absorpt_correction_T_min  0,380292
_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   4
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.715
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.03
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+5.3316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                2864
_reflns_number_total             3425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701795y-file006_1.cif
_cod_data_source_block           irpza
_cod_database_code               4304314