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_2021837
_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          '[Ir (C8 H12) (C32 H42 N6)] Br, C H2 Cl2'
_chemical_formula_moiety         'C40 H54 Ir N6 +, Br -, C H2 Cl2'
_chemical_formula_sum            'C41 H56 Br Cl2 Ir N6 O'
_chemical_formula_weight         991.92
_chemical_name_systematic
;[(1,2,5,6-\h)-Cycloocta-1,5-diene](5,16-dibenzyl-1,5,9,12,16,20-hexaazatricyclo[18.2.1.1^9,12^]tetracosa-10,21-dien-21,22-diylidene)iridium(I)
bromide dichloromethane monosolvate
;
_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-2018/3
_cell_angle_alpha                91.6088(18)
_cell_angle_beta                 95.5859(19)
_cell_angle_gamma                110.4270(16)
_cell_formula_units_Z            2
_cell_length_a                   10.3943(4)
_cell_length_b                   13.6413(6)
_cell_length_c                   15.8517(7)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.35
_cell_measurement_theta_min      2.34
_cell_volume                     2091.66(16)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2010)
;
_computing_publication_material
;
SHELXTL (Bruker, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44172
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5165
_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    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.714
_refine_diff_density_min         -4.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         11734
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                11240
_reflns_number_total             11734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3185sup1.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2091.66(15)
_cod_database_code               2021837
_shelx_estimated_absorpt_t_min   0.407
_shelx_estimated_absorpt_t_max   0.794
_shelx_hkl_checksum              1010
_shelx_res_checksum              97477
_shelx_fab_checksum              7867
_cod_database_fobs_code 2021837