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_4304316
_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             2007-11-24T18:51:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.4071(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.87890(17)
_cell_length_b                   13.626(2)
_cell_length_c                   20.3750(4)
_cell_measurement_reflns_used    7412
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3607
_cell_measurement_theta_min      3.7545
_cell_measurement_wavelength     0.71073
_cell_volume                     2465.0(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_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_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.917
_diffrn_orient_matrix_UB_11      -0.0778435785
_diffrn_orient_matrix_UB_12      -0.0108750532
_diffrn_orient_matrix_UB_13      0.002277524
_diffrn_orient_matrix_UB_21      -0.0017046748
_diffrn_orient_matrix_UB_22      0.021574505
_diffrn_orient_matrix_UB_23      0.0316229139
_diffrn_orient_matrix_UB_31      -0.0175215197
_diffrn_orient_matrix_UB_32      0.0460827556
_diffrn_orient_matrix_UB_33      -0.0142768251
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16382
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         31.5
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    5.719
_exptl_absorpt_correction_T_max  0.32
_exptl_absorpt_correction_T_min  0.15892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                4959
_reflns_number_total             7502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701795y-file007.cif
_cod_data_source_block           irptaf
_cod_database_code               4304316