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_2242510
_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) Cl H] Cl, 5H2 O'
_chemical_formula_moiety         '[(C51 H45 P4)Ir(H)Cl], Cl, 5(H2 O)'
_chemical_formula_sum            'C51 H56 Cl3 Ir O5 P4'
_chemical_formula_weight         1171.38
_chemical_name_systematic
'Dichloridohydrido(1,1,3,3,5,5,7,7-octaphenyl-1,7-diphospha-3,5-diphosphoniaheptan-4-yl)iridium(III) chloride pentahydrate'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.381(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6532(8)
_cell_length_b                   21.8847(12)
_cell_length_c                   19.9228(12)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.7
_cell_volume                     5443.1(6)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_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
;
<i>SHELXT2014/4</i> (Sheldrick, 2015a; Ruf & Noll, 2014)
;
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104100
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.930
_diffrn_reflns_theta_min         2.130
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.865
_refine_ls_extinction_coef       0.00056(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
(SHELXL-2014/7; Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         10577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+9.2728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                9522
_reflns_number_total             10577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5440sup1.cif
_cod_data_source_block           3
_cod_database_code               2242510
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.789
_shelx_hkl_checksum              56446
_shelx_res_checksum              61850
_cod_database_fobs_code 2242510