Selective low-temperature syntheses of facial and meridional tris-cyclometalated iridium(III) complexes.
McGee, Kari A.; Mann, Kent R.; Inorganic chemistry 46 (2007) 7800–7809; doi:10.1021/ic700440c

data_4339822
_publ_section_title
;
 Selective low-temperature syntheses of facial and meridional
 tris-cyclometalated iridium(III) complexes.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7800
_journal_page_last               7809
_journal_paper_doi               10.1021/ic700440c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C27 H19 Ir N3 S3, F6 P'
_chemical_formula_sum            'C27 H19 F6 Ir N3 P S3'
_chemical_formula_weight         818.80
_chemical_name_common            04085
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            36
_cell_length_a                   20.8082(18)
_cell_length_b                   20.8082
_cell_length_c                   71.402(7)
_cell_measurement_reflns_used    2066
_cell_measurement_temperature    173(2)
_cell_volume                     26774(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, BRuker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -84
_diffrn_reflns_number            27208
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    4.813
_exptl_absorpt_correction_T_max  0.790000
_exptl_absorpt_correction_T_min  0.461158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14256
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         5286
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0519P)^2^+107.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3602
_reflns_number_total             5286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tris_ir_cifs_revised.cif
_cod_data_source_block           04085z
_cod_original_cell_volume        26774(3)
_cod_original_sg_symbol_H-M      R-3C
_cod_database_code               4339822