Synthesis and structural characterization of iridium(I) complexes of 20-membered macrocyclic rings bearing chelating bis(N-heterocyclic carbene) ligands
Thapa, Rajesh; Kilyanek, Stefan M.; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619015006

data_2021836
_publ_section_title
;
 Synthesis and structural characterization of iridium(I) complexes of
 20-membered macrocyclic rings bearing chelating bis(N-heterocyclic
 carbene) ligands
;
_journal_coeditor_code           KY3185
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619015006
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C32 H44 N6 2+, 2P F6 -'
_chemical_formula_moiety         'C32 H44 N6 2+, 2(F6 P -)'
_chemical_formula_sum            'C32 H44 F12 N6 P2'
_chemical_formula_weight         802.67
_chemical_name_systematic
'5,16-Dibenzyl-1\l^5^,5,9,12\l^5^,16,20-hexaazatricyclo[18.2.1.1^9,12^]tetracosa-1(23),10,12(24),21-tetraene-1,12-diium bis(hexafluorophosphate)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                95.133(17)
_cell_angle_beta                 97.423(17)
_cell_angle_gamma                100.660(17)
_cell_formula_units_Z            2
_cell_length_a                   9.290(12)
_cell_length_b                   11.228(14)
_cell_length_c                   18.00(2)
_cell_measurement_reflns_used    4108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.26
_cell_volume                     1817(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28213
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.862
_diffrn_reflns_theta_min         1.149
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.474
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                4809
_reflns_number_total             8188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3185sup1.cif
_cod_data_source_block           1c
_cod_database_code               2021836
_cod_database_fobs_code          2021836
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              38103
_shelx_res_checksum              76042