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_4304315
_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         'C13 H18 N3 O2 P1'
_chemical_formula_sum            'C13 H18 N3 O2 P'
_chemical_formula_weight         279.27
_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             2007-07-27T16:07:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.97(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.485(3)
_cell_length_b                   11.337(4)
_cell_length_c                   11.004(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.49
_cell_measurement_theta_min      4.04
_cell_measurement_wavelength     0.71073
_cell_volume                     1295.4(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.090667
_diffrn_orient_matrix_UB_12      0.025413
_diffrn_orient_matrix_UB_13      0.027933
_diffrn_orient_matrix_UB_21      -0.031693
_diffrn_orient_matrix_UB_22      0.079137
_diffrn_orient_matrix_UB_23      0.022649
_diffrn_orient_matrix_UB_31      -0.006988
_diffrn_orient_matrix_UB_32      -0.029523
_diffrn_orient_matrix_UB_33      0.084422
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.1644
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2408
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        14
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.193
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+3.0016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                1236
_reflns_number_total             2277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701795y-file006_2.cif
_cod_data_source_block           pzao
_cod_database_code               4304315