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_2242488
_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 (C O) (C51 H44 P4)] Cl, 3C H2 Cl2'
_chemical_formula_sum            'C55 H51 Cl8 Ir O P4'
_chemical_formula_weight         1327.64
_chemical_name_systematic
;
(Bis{[(diphenylphosphanyl)methyl]diphenylphosphanylidene}methane-\
\k^3^<i>P</i>,<i>C</i>,<i>P</i>')carbonylchloridohydridoiridium(III) chloride
dichloromethane trisolvate
;
_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                 91.7000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3477(2)
_cell_length_b                   24.7472(5)
_cell_length_c                   19.0123(3)
_cell_measurement_reflns_used    76576
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     5807.05(18)
_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_molecular_graphics
;
CHEMDRAW (Cambridge Soft, 2001)
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33007
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.815
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.911
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10203
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+13.9388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                8088
_reflns_number_total             10203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb2007sup1.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2242488
_cod_database_fobs_code 2242488