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_2021838
_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          '[Ir2 Br2 (C8 H12)2 (C40 H46 N6)]'
_chemical_formula_moiety         'C56 H70 Br2 Ir2 N6'
_chemical_formula_sum            'C56 H70 Br2 Ir2 N6'
_chemical_formula_weight         1371.40
_chemical_name_systematic
'[\m-5,20-dibenzyl-1,5,9,16,20,24-hexaazapentacyclo[22.6.1.1^9,16^.0^10,15^.0^25,30]dotriaconta-10(15),11,13,25(30),26,28-hexaene-31,32-diylidene]bis{bromido[(1,2,5,6-\h)-cycloocta-1,5-diene]iridium(I)}'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.6186(5)
_cell_length_b                   27.2390(11)
_cell_length_c                   30.2461(11)
_cell_measurement_reflns_used    9077
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.30
_cell_volume                     10396.1(7)
_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
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Photon II cpad'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            58196
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    6.695
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.678
_refine_diff_density_min         -3.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         11002
_refine_ls_number_restraints     1671
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0774
_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^)+(0.1000P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                8220
_reflns_number_total             11002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3185sup1.cif
_cod_data_source_block           2b
_cod_database_code               2021838
_shelx_estimated_absorpt_t_min   0.234
_shelx_estimated_absorpt_t_max   0.610
_shelx_hkl_checksum              16281
_shelx_res_checksum              5218
_cod_database_fobs_code 2021838