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_4319197
_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_compound_source        'Prof. D. Krogstad - University of the South'
_chemical_formula_sum            'C25 H54 Cl Ir N12 O4 P4'
_chemical_formula_weight         938.33
_chemical_name_common            98324a
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3619(4)
_cell_length_b                   14.0345(3)
_cell_length_c                   24.1575(5)
_cell_measurement_temperature    173(2)
_cell_volume                     6903.5(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50778
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.184
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.454
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_obs          0.0246
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+7.3789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0605
_refine_ls_wR_factor_obs         0.0574
_reflns_number_observed          4805
_reflns_number_total             6115
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000501l_1.cif
_cod_data_source_block           3
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+7.3789P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+7.3789P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319197