2-Pyridine cyclic triimidazole as a chelating and bridging ligand in mono- and hexa-nuclear Re(i) complexes with emissive properties in solution and in the solid state
Malpicci, Daniele; Maver, Daniele; Maggioni, Daniela; Mercandelli, Pierluigi; Carlucci, Lucia; Cariati, Elena; Mussini, Patrizia; Panigati, Monica; New Journal of Chemistry 47 (2023) 21463–21474; doi:10.1039/D3NJ02823B

data_7062846
_publ_section_title
;
 2-Pyridine cyclic triimidazole as a chelating and bridging ligand in
 mono- and hexa-nuclear Re(i) complexes with emissive properties in
 solution and in the solid state
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21463
_journal_page_last               21474
_journal_paper_doi               10.1039/D3NJ02823B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C46 H18 Cl6 N14 O18 Re6, 4(C6 H14)'
_chemical_formula_sum            'C70 H74 Cl6 N14 O18 Re6'
_chemical_formula_weight         2729.33
_chemical_name_systematic
'octadecacarbonyl-hexachloro-bis[3-(pyridin-2-yl-\kN)tri-imidazo[1,2-a:1',2'-c:1'',2''-e][1,3,5]triazine-\kN^5^]-hexarhenium n-hexane solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-10-21 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.310(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0102(15)
_cell_length_b                   35.458(4)
_cell_length_c                   18.735(2)
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.677
_cell_measurement_theta_min      2.319
_cell_volume                     8728.4(17)
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SIR-2014
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.5\% \w steps,
collecting 6 sets of 360 frames each, at 30 s exposure, keeping the detector
at \q = 30\% and at 5.0 cm from the sample.
;
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.149
_exptl_absorpt_coefficient_mu    8.541
_exptl_absorpt_correction_T_max  0.7840
_exptl_absorpt_correction_T_min  0.4909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1
Reflections employed for parameter determination: 78426
Maximum odd and even orders for spherical harmonics: 7 and 8
Effective data to parameter ratio: 26.32
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             5152
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane into a
dichloromethane solution at 248 K.
;
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.816
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 6980 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         17863
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0425P)^2^+7.6721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15878
_reflns_number_total             17863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02823b3.cif
_cod_data_source_block           1008
_cod_depositor_comments
'Adding full bibliography for 7062845--7062846.cif.'
_cod_original_cell_volume        8728.5(16)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7062846
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.144
_shelx_estimated_absorpt_t_max   0.784
_shelx_res_checksum              87879