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_4339820
_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         'C22 H18 Ir N4 S2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C23 H20 Cl2 F6 Ir N4 P S2'
_chemical_formula_weight         824.62
_chemical_name_common            04011
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                98.724(2)
_cell_angle_beta                 105.480(2)
_cell_angle_gamma                102.992(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4639(13)
_cell_length_b                   13.114(2)
_cell_length_c                   13.816(2)
_cell_measurement_reflns_used    1011
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.27
_cell_volume                     1403.0(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12046
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    5.216
_exptl_absorpt_correction_T_max  0.3536
_exptl_absorpt_correction_T_min  0.227302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.402
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+4.7535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                4520
_reflns_number_total             4952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tris_ir_cifs_revised.cif
_cod_data_source_block           04011m
_cod_original_cell_volume        1403.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339820