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_4304156
_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         'C22 H26 Ir N6 1+, F6 P 1-'
_chemical_formula_sum            'C22 H26 F6 Ir N6 P'
_chemical_formula_weight         711.66
_chemical_name_systematic
; 
(2,2'-Bipyridine)(5-methyltetrazolato-\kN^2^)
(\h^5^-pentamethylcyclopentadienyl)iridium(III) Hexafluorophosphate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.760(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8503(7)
_cell_length_b                   28.408(2)
_cell_length_c                   9.8675(5)
_cell_measurement_reflns_used    11404
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2475.5(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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22766
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    5.527
_exptl_absorpt_correction_T_max  0.4911
_exptl_absorpt_correction_T_min  0.3387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0078P)^2^+11.1232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4925
_reflns_number_total             5564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic701631k-file003_1.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        2475.6(3)
_cod_database_code               4304156