Elegant Approach to the Synthesis of a Unique Heteroleptic Cyclometalated Iridium(III)-Polyoxometalate Conjugate
Matt, Benjamin; Moussa, Jamal; Chamoreau, Lise-Marie; Afonso, Carlos; Proust, Anna; Amouri, Hani; Izzet, Guillaume; Organometallics 31 (2012) 35–; doi:10.1021/om200910p

data_4067917
_publ_section_title
;
 Elegant Approach to the Synthesis of a Unique Heteroleptic Cyclometalated
 Iridium(III)-Polyoxometalate Conjugate
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              35
_journal_paper_doi               10.1021/om200910p
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety
'C33 H28 Ir N3 O2 Si, 0.5 (C4 H10 O), 0.5 (C3 H6 O)'
_chemical_formula_sum            'C36.5 H36 Ir N3 O3 Si'
_chemical_formula_weight         784.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                94.7370(10)
_cell_angle_beta                 93.0460(10)
_cell_angle_gamma                104.7840(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4581(3)
_cell_length_b                   12.0415(3)
_cell_length_c                   13.7808(3)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.3
_cell_volume                     1667.28(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34796
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.080
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9744
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0176P)^2^+1.1413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                9077
_reflns_number_total             9744
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200910p_si_002.cif
_cod_data_source_block           jm11_23_0m
_cod_original_formula_sum        'C36.50 H36 Ir N3 O3 Si'
_cod_database_code               4067917