Synthesis and Reactivity of Ir(I) and Ir(III) Complexes with MeNH2, Me2C=NR (R = H, Me), C,N-C6H4{C(Me)=N(Me)}-2, and N,N'-RN=C(Me)CH2C(Me2)NHR (R = H, Me) Ligands
José Vicente; María Teresa Chicote; Inmaculada Vicente-Hernández; Delia Bautista; Inorganic Chemistry 47 (2008) 9592–9605; doi:10.1021/ic801184v

data_4306334
_publ_section_title
;
Synthesis and Reactivity of Ir(I) and Ir(III) Complexes with MeNH2,
Me2C=NR (R = H, Me), C,N-C6H4{C(Me)=N(Me)}-2,
and N,N'-RN=C(Me)CH2C(Me2)NHR (R = H, Me) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9592
_journal_page_last               9605
_journal_paper_doi               10.1021/ic801184v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C10 H18 Cl2 Ir N'
_chemical_formula_weight         415.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.791(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6828(6)
_cell_length_b                   7.7401(5)
_cell_length_c                   19.4092(13)
_cell_measurement_reflns_used    8679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.40
_cell_volume                     1276.89(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14215
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    10.839
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.4776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    'NH3 free with sadi,methyls rigid'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0211P)^2^+2.7931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                2875
_reflns_number_total             2964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801184v_si_001_1.cif
_cod_data_source_block           ivc33s
_cod_database_code               4306334