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_2021424
_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 (C N) Cl H (C51 H44 P4)], C2 H3 N'
_chemical_formula_moiety         'C52 H45 Cl Ir N P4, C2 H3 N'
_chemical_formula_sum            'C54 H48 Cl Ir N2 P4'
_chemical_formula_weight         1076.47
_chemical_name_systematic
;Chloridocyanidohydrido(1,1,3,3,5,5,7,7-octaphenyl-1,3\l^5^,5\l^4^,7-tetraphospha-\k^2^<i>P</i>^1^,<i>P</i>^7^-hept-3-en-4-yl)iridium(III)
acetonitrile monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.8030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3264(3)
_cell_length_b                   13.6459(2)
_cell_length_c                   19.3010(4)
_cell_measurement_reflns_used    52211
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     4724.74(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0859
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25915
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.396
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.558
_refine_diff_density_min         -1.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0210P)^2^+3.0711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                6345
_reflns_number_total             8317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5464sup1.cif
_cod_data_source_block           1b
_cod_database_code               2021424
_shelx_hkl_checksum              59066
_shelx_res_checksum              48957
_cod_database_fobs_code 2021424