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_4304161
_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
'C38 H42 Ir2 N2 S2 2+, 2(F6 P 1-), 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H43.5 F12 Ir2 N2.5 P2 S2'
_chemical_formula_weight         1285.72
_chemical_name_systematic
; 
Bis[\m-8-quinolinethiolato-\k^2^S,N:\kS]bis[(\h^5^-pentamethylcyclopentadienyl) 
iridium(III)] Bis(hexafluorophosphate) Hemi(acetonitrile) Solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.9890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2968(4)
_cell_length_b                   12.9142(4)
_cell_length_c                   23.2092(7)
_cell_measurement_reflns_used    23813
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     4206.6(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40097
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    6.583
_exptl_absorpt_correction_T_max  0.5055
_exptl_absorpt_correction_T_min  0.3527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment
;
constr except for those of the solvated acetonitrile molecule
which were not included
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+8.7334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0497
_reflns_number_gt                8503
_reflns_number_total             9574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic701631k-file003_6.cif
_cod_data_source_block           complex8
_cod_original_formula_sum        'C39 H43.50 F12 Ir2 N2.50 P2 S2'
_cod_database_code               4304161