ONO Dianionic Pincer-Type Ligand Precursors for the Synthesis of σ,π-Cyclooctenyl Iridium(III) Complexes: Formation Mechanism and Coordination Chemistry
Nguyen, Duc Hanh; Greger, Ingo; Pérez-Torrente, Jesús J.; Jiménez, M. Victoria; Modrego, F. Javier; Lahoz, Fernando J.; Oro, Luis A.; Organometallics 32 (2013) 6903–; doi:10.1021/om400767d

data_4081905
_publ_section_title
;
 ONO Dianionic Pincer-Type Ligand Precursors for the Synthesis of
 \s,\p-Cyclooctenyl Iridium(III) Complexes: Formation Mechanism and
 Coordination Chemistry
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6903
_journal_paper_doi               10.1021/om400767d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C40 H38 Ir N O4 P2'
_chemical_formula_sum            'C40 H38 Ir N O4 P2'
_chemical_formula_weight         850.85
_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                111.006(3)
_cell_angle_beta                 95.558(3)
_cell_angle_gamma                103.966(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6225(13)
_cell_length_b                   13.0524(17)
_cell_length_c                   15.245(2)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.57
_cell_measurement_theta_min      2.22
_cell_volume                     1698.7(4)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18343
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.068
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.7341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.  
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.107
_refine_diff_density_min         -2.072
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4921
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400767d_si_002.cif
_cod_data_source_block           compound_1_dppm
_cod_original_cell_volume        1698.8(4)
_cod_database_code               4081905