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_1565755
_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 N12 Re6 Se8, 4(C3 H4 N2), 2(Br)'
_chemical_formula_sum            'C30 H40 Br2 N20 Re6 Se8'
_chemical_formula_weight         2589.52
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                74.6620(10)
_cell_angle_beta                 64.3250(10)
_cell_angle_gamma                88.030(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4459(6)
_cell_length_b                   11.5271(6)
_cell_length_c                   11.5348(5)
_cell_measurement_reflns_used    6238
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.55
_cell_volume                     1317.12(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11457
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.840
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.265
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.4893
_refine_diff_density_max         2.134
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.00031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4891
_reflns_number_total             5785
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            2Br24pzH.cif
_cod_data_source_block           win094
_cod_database_code               1565755
_shelx_estimated_absorpt_t_min   0.103
_shelx_estimated_absorpt_t_max   0.189
_shelx_res_checksum              44631
_shelx_hkl_checksum              32113