Synthesis and Characterization of Iridium 1,3,5-Triaza-7-phosphaadamantane (PTA) Complexes. X-ray Crystal and Molecular Structures of [Ir(PTA)4(CO)]Cl and [Ir(PTAH)3(PTAH2)(H)2]Cl6
Don A. Krogstad; Jason A. Halfen; Tracy J. Terry; Victor G. Young; Inorganic Chemistry 40 (2001) 463–471; doi:10.1021/ic000501l

data_4319198
_publ_section_title
;
 Synthesis and Characterization of Iridium
 1,3,5-Triaza-7-phosphaadamantane (PTA) Complexes. X-ray Crystal and
 Molecular Structures of [Ir(PTA)4(CO)]Cl and [Ir(PTAH)3(PTAH2)(H)2]Cl6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              463
_journal_page_last               471
_journal_paper_doi               10.1021/ic000501l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H72 Cl7 Ir N12 O7 P4'
_chemical_formula_weight         1205.17
_chemical_name_common            0001
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.004(1)
_cell_angle_beta                 71.605(1)
_cell_angle_gamma                69.177(1)
_cell_formula_units_Z            2
_cell_length_a                   12.4432(9)
_cell_length_b                   12.5921(9)
_cell_length_c                   16.3231(12)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_volume                     2244.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10124
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.312
_refine_diff_density_min         -3.772
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         10124
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+20.1769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                9392
_reflns_number_total             10124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000501l_2.cif
_cod_data_source_block           5
_cod_database_code               4319198