Structural Versatility of 5-Methyltetrazolato Complexes of (η5-Pentamethylcyclopentadienyl)iridium(III) Incorporating 2,2'-Bipyridine, N,N-Dimethyldithiocarbamate, or 2-Pyridinethiolate Ligands
Mai Kotera; Yusuke Sekioka; Takayoshi Suzuki; Inorganic Chemistry 47 (2008) 3498–3508; doi:10.1021/ic701631k

data_4304163
_publ_section_title
;
Structural Versatility of 5-Methyltetrazolato Complexes of
(\h5-Pentamethylcyclopentadienyl)iridium(III) Incorporating
2,2'-Bipyridine, N,N-Dimethyldithiocarbamate, or 2-Pyridinethiolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3498
_journal_page_last               3508
_journal_paper_doi               10.1021/ic701631k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C26 H39 Ir2 N12 1+, F6 P 1-, 2(H2 O)'
_chemical_formula_sum            'C26 H43 F6 Ir2 N12 O2 P'
_chemical_formula_weight         1085.09
_chemical_name_systematic
; 
Tris[\m-5-methyltetrazolato-\kN^2^:\kN^3^]
bis[(\h^5^-pentamethylcyclopentadienyl)iridium(III)] 
Hexafluorophosphate Dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                87.023(2)
_cell_angle_beta                 67.242(2)
_cell_angle_gamma                83.122(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5401(10)
_cell_length_b                   11.7447(12)
_cell_length_c                   14.9334(16)
_cell_measurement_reflns_used    10971
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     1853.0(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'CrystalStructure 3.8'
_computing_molecular_graphics    'ORTEP-3 for win'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16153
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    7.290
_exptl_absorpt_correction_T_max  0.4077
_exptl_absorpt_correction_T_min  0.3234
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.730
_refine_diff_density_min         -3.898
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment
;
constr except for those of the solvated water molecules
which were not included
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+43.6314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                7378
_reflns_number_total             8310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic701631k-file003_8.cif
_cod_data_source_block           complex10
_cod_database_code               4304163