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_2242511
_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 (C O)] Cl, 2C H4 O, H2 O'
_chemical_formula_moiety
'[(C51 H44 P4)Ir(H)(CO)Cl], Cl, 2(C H3 O H), (H2 O)'
_chemical_formula_sum            'C54 H56 Cl2 Ir O4 P4'
_chemical_formula_weight         1154.96
_chemical_name_systematic
'Carbonylchloridohydrido(1,1,3,3,5,5,7,7-octaphenyl-1,5\l^5^,7-triphospha-3-phosphoniahept-4-en-4-yl)iridium(III) chloride--methanol--water (1/2/1)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.5350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5929(2)
_cell_length_b                   23.2803(4)
_cell_length_c                   19.7488(4)
_cell_measurement_reflns_used    183501
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     5520.66(17)
_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
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      233(2)
_diffrn_detector_area_resol_mean 9.4
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32186
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.391
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.451
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9675
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+16.7009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                8070
_reflns_number_total             9675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5440sup1.cif
_cod_data_source_block           4
_cod_database_code               2242511
_shelx_estimated_absorpt_t_min   0.604
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              16504
_shelx_res_checksum              74144
_cod_database_fobs_code 2242511