Crystal structures of two PCN pincer iridium complexes and one PCP pincer carbodiphosphorane iridium intermediate: substitution of one phosphine moiety of a carbodiphosphorane by an organic azide
Partl, Gabriel Julian; Nussbaumer, Felix; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Peringer, Paul; Acta Crystallographica Section E Crystallographic Communications 75 (2019) 75–; doi:10.1107/S2056989018017644

data_2021425
_publ_section_title
;
 Crystal structures of two PCN pincer iridium complexes and one PCP pincer
 carbodiphosphorane iridium intermediate: substitution of one phosphine
 moiety of a carbodiphosphorane by an organic azide
;
_journal_coeditor_code           SU5464
_journal_issue                   1
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              75
_journal_paper_doi               10.1107/S2056989018017644
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Ir (C25 H22 P2) (C32 H26 Cl N3 P2)] Cl, 0.5C7 H8, 1.5C H2 Cl2'
_chemical_formula_moiety
'C57 H48 Cl Ir N3 P4 +, Cl -, 0.5(C7 H8), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C62 H55 Cl5 Ir N3 P4'
_chemical_formula_weight         1335.42
_chemical_name_systematic
'[7-(4-Chlorophenyl)-1,1,3,3-tetraphenyl-5,6,7-triaza-\k<i>N</i>^7^-1,3\l^4^-diphospha-\k<i>P</i>^1^-hepta-4,6-dien-4-yl][methylenebis(diphenylphosphine)-\k^2^<i>P</i>,<i>P</i>']iridium(I) chloride--dichloromethane--toluene (2/3/1)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.1283(3)
_cell_length_b                   19.0989(2)
_cell_length_c                   23.6339(2)
_cell_measurement_reflns_used    221720
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.0
_cell_volume                     12696.6(2)
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>,  2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      233(2)
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73594
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.869
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             5360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.728
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11155
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+44.6168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                9002
_reflns_number_total             11155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5464sup1.cif
_cod_data_source_block           2
_cod_database_code               2021425
_shelx_hkl_checksum              43345
_shelx_res_checksum              92725
_cod_database_fobs_code 2021425