Synthesis and luminescence properties of apically homoleptic octahedral rhenium clusters with pyrazole and 3,5-dimethylpyrazole
Konovalov, Dmitriy I.; Ivanov, Anton A.; Vorotnikov, Yuri A.; Brylev, Konstantin A.; Eltsov, Ilia V.; Kuratieva, Natalia V.; Kitamura, Noboru; Mironov, Yuri V.; Shestopalov, Michael A.; Inorganica Chimica Acta 498 (2019) 119128–; doi:10.1016/j.ica.2019.119128

data_1565756
_publ_section_title
;
 Synthesis and luminescence properties of apically homoleptic octahedral
 rhenium clusters with pyrazole and 3,5-dimethylpyrazole
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119128
_journal_paper_doi               10.1016/j.ica.2019.119128
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C18 H24 Cl2 N12 Re6 Se8'
_chemical_formula_sum            'C18 H24 Cl2 N12 Re6 Se8'
_chemical_formula_weight         2228.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.722(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1562(13)
_cell_length_b                   16.637(2)
_cell_length_c                   20.729(3)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.30
_cell_volume                     3792.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36128
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.404
_diffrn_reflns_theta_min         1.578
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.929
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.903
_exptl_crystal_description       prism
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.062
_refine_diff_density_min         -3.296
_refine_diff_density_rms         0.354
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0332P)^2^+51.6973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7400
_reflns_number_total             9411
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            2Cl2.cif
_cod_data_source_block           win123
_cod_original_cell_volume        3792.1(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565756
_shelx_estimated_absorpt_t_min   0.085
_shelx_estimated_absorpt_t_max   0.295
_shelx_res_checksum              99433
_shelx_hkl_checksum              86310