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_1565758
_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         'C30 H48 N12 Re6 Se8, 2(C5 H8 N2), 2(Cl)'
_chemical_formula_sum            'C40 H64 Cl2 N16 Re6 Se8'
_chemical_formula_weight         2588.85
_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                 92.312(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0119(14)
_cell_length_b                   18.418(2)
_cell_length_c                   13.5776(16)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.21
_cell_volume                     3001.4(6)
_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      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35241
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.634
_diffrn_reflns_theta_min         2.025
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.036
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.865
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0186
_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^)+(0.0196P)^2^+0.2602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0431
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5864
_reflns_number_total             6901
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            4Cl22Me2pzH.cif
_cod_data_source_block           win127
_cod_original_cell_volume        3001.3(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565758
_shelx_estimated_absorpt_t_min   0.171
_shelx_estimated_absorpt_t_max   0.343
_shelx_res_checksum              18928
_shelx_hkl_checksum              50656