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_2021426
_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) (C23 H22 P2) (C34 H26 Cl N3 P2)], 2C H4 O'
_chemical_formula_moiety         'C58 H48 Cl Ir N4 P4, 2(C H4 O)'
_chemical_formula_sum            'C60 H56 Cl Ir N4 O2 P4'
_chemical_formula_weight         1216.61
_chemical_name_systematic
;{4-[3-(4-Chlorophenyl)triazenido-\k<i>N</i>^3^]-1,1,3,3-tetraphenyl-1,3\l^5^-diphospha-\k<i>P</i>^1^-but-2-en-4-yl}cyanido[methylenebis(diphenylphosphine)-\k^2^<i>P</i>,<i>P</i>']iridium(III)
methanol disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                98.4750(10)
_cell_angle_beta                 93.1220(10)
_cell_angle_gamma                109.3360(10)
_cell_formula_units_Z            2
_cell_length_a                   11.16830(10)
_cell_length_b                   12.7805(2)
_cell_length_c                   20.0591(3)
_cell_measurement_reflns_used    31262
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2655.76(7)
_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      223(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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20072
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0184P)^2^+2.0572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                9895
_reflns_number_total             10396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5464sup1.cif
_cod_data_source_block           3
_cod_original_cell_volume        2655.75(6)
_cod_database_code               2021426
_shelx_hkl_checksum              16277
_shelx_res_checksum              84758
_cod_database_fobs_code 2021426