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_2242509
_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 H44 P4) Cl H] Cl, C3 H6 O'
_chemical_formula_moiety         '[(C51 H44 P4)Ir(H)Cl], Cl, (CH3)2 C O'
_chemical_formula_sum            'C54 H51 Cl2 Ir O P4'
_chemical_formula_weight         1102.93
_chemical_name_systematic
'Dichloridohydrido(1,1,3,3,5,5,7,7-octaphenyl-1,5\l^5^,7-triphospha-3-phosphoniahept-4-en-4-yl)iridium(III) acetone monosolvate'
_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                 101.586(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7964(4)
_cell_length_b                   13.7444(2)
_cell_length_c                   18.8487(4)
_cell_measurement_reflns_used    78297
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      1.0
_cell_volume                     4770.25(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0825
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27235
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.805
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0337P)^2^+5.1790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                6069
_reflns_number_total             8407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5440sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               2242509
_cod_database_fobs_code 2242509