Triply cyclometalated trinuclear iridium(iii) and trinuclear palladium(ii) complexes with a tri-mesoionic carbene ligand.
Maity, Ramananda; Mekic, Amel; van der Meer, Margarethe; Verma, Amit; Sarkar, Biprajit; Chemical communications (Cambridge, England) 51 (2015) 15106–15109; doi:10.1039/c5cc05506g

data_7117880
_publ_section_title
;
 Triply cyclometalated trinuclear iridium(iii) and trinuclear
 palladium(ii) complexes with a tri-mesoionic carbene ligand.
;
_journal_issue                   82
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15106
_journal_page_last               15109
_journal_paper_doi               10.1039/c5cc05506g
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C113.67 H108 Cl11 I12 N24 Pd6'
_chemical_formula_weight         4361.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-27 deposited with the CCDC.
2015-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   35.2807(14)
_cell_length_b                   35.2807(14)
_cell_length_c                   10.4598(4)
_cell_measurement_reflns_used    4102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.31
_cell_volume                     11275.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega + phi 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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            60558
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.412
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6171
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.386
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5059
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0455P)^2^+223.0825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                4102
_reflns_number_total             5059
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc05506g2.cif
_cod_data_source_block           bip27
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7117880