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_4306335
_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            'C19 H36 Cl2 Ir N3'
_chemical_formula_weight         569.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 99.821(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6457(6)
_cell_length_b                   13.6922(7)
_cell_length_c                   15.9691(8)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.51
_cell_volume                     2293.6(2)
_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      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.946
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25654
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    6.061
_exptl_absorpt_correction_T_max  0.6115
_exptl_absorpt_correction_T_min  0.2724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment
'NH free with SADI, rigid methyls others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5278
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.0446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                4830
_reflns_number_total             5278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801184v_si_001_2.cif
_cod_data_source_block           ivc44s
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4306335