Crystal structure of an iridium(III) complex of the [C(dppm)~2~] PCP pincer ligand system and its conjugate CH acid form
Reitsamer, Christian; Schlapp-Hackl, Inge; Partl, Gabriel; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Peringer, Paul; Acta Crystallographica Section E 74 (2018) 620–624; doi:10.1107/S2056989018004905

data_2242489
_publ_section_title
;
 Crystal structure of an iridium(III) complex of the [C(dppm)~2~] PCP
 pincer ligand system and its conjugate CH acid form
;
_journal_coeditor_code           EB2007
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              620
_journal_page_last               624
_journal_paper_doi               10.1107/S2056989018004905
_journal_volume                  74
_journal_year                    2018
_chemical_formula_moiety
'[Ir Cl H (C51 H44 P4) (C O)] Cl2, 2 H Cl, 5.5H2 O'
_chemical_formula_sum            'C52 H59 Cl5 Ir O6.5 P4'
_chemical_formula_weight         1281.32
_chemical_name_systematic
;(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}methane(1+)-\k^3^<i>P</i>,<i>C</i>,<i>P</i>')carbonylchloridohydridoiridium(III)
dichloride--hydrochloric acid--water (1/2/5.5)
;
_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                 98.7810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.7138(2)
_cell_length_b                   22.7327(2)
_cell_length_c                   25.3120(3)
_cell_measurement_reflns_used    114911
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.0
_cell_volume                     11210.6(2)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT Nonius, 1999
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS-97 (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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68943
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.031
_refine_diff_density_min         -0.994
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1268
_refine_ls_number_reflns         22078
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+17.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                17290
_reflns_number_total             22078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb2007sup1.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C52 H59 Cl5 Ir O6.50 P4'
_cod_database_code               2242489
_cod_database_fobs_code 2242489