Crystal structures of four new iridium complexes, each containing a highly flexible carbodiphosphorane PCP pincer ligand
Partl, Gabriel Julian; Nussbaumer, Felix; Schlapp-Hackl, Inge; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Peringer, Paul; Acta Crystallographica Section E 74 (2018) 846–852; doi:10.1107/S2056989018007569

data_2242508
_publ_section_title
;
 Crystal structures of four new iridium complexes, each containing a
 highly flexible carbodiphosphorane PCP pincer ligand
;
_journal_coeditor_code           SU5440
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              846
_journal_page_last               852
_journal_paper_doi               10.1107/S2056989018007569
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Ir (C51 H45 P4) (C8 H12)] (C F3 S O3)2, C H3 C O2 C2 H5, C H2 Cl2'
_chemical_formula_moiety
'[(C8 H12) Ir (C51 H45 P4)], 2(F3 C S O3), C H3 C O2 C2 H5, C H2 Cl2'
_chemical_formula_sum            'C66 H67 Cl2 F6 Ir O8 P4 S2'
_chemical_formula_weight         1553.30
_chemical_name_systematic
'(Cycloocta-1,5-diene)(1,1,3,3,5,5,7,7-octaphenyl-1,7-diphospha-3,5-diphosphoniaheptan-4-yl)iridium(I) bis(trifluoromethanesulfonate)--ethyl acetate--dichloromethane (1/1/1)'
_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                68.9490(10)
_cell_angle_beta                 74.4260(10)
_cell_angle_gamma                70.2560(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3105(2)
_cell_length_b                   14.3109(3)
_cell_length_c                   19.8482(3)
_cell_measurement_reflns_used    37798
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     3274.11(10)
_computing_cell_refinement
;
COLLECT (Nonius, 1998)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20473
_diffrn_reflns_theta_full        24.84
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.682
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         11235
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+2.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                10195
_reflns_number_total             11235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5440sup1.cif
_cod_data_source_block           1b
_cod_original_cell_volume        3274.10(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2242508
_cod_database_fobs_code 2242508