Dinuclear Rhenium pyridazine complexes containing bridging chalcogenide anions: synthesis, characterization and computational study
Veronese, Lorenzo; Quartapelle Procopio, Elsa; Maggioni, Daniela; Mercandelli, Pierluigi; Panigati, Monica; New J. Chem.  (2017) –; doi:10.1039/C7NJ02548C

data_7056552
_publ_section_title
;
 Dinuclear Rhenium pyridazine complexes containing bridging chalcogenide
 anions: synthesis, characterization and computational study
;
_journal_name_full               'New J. Chem.'
_journal_paper_doi               10.1039/C7NJ02548C
_journal_year                    2017
_chemical_formula_moiety         'C22 H14 N2 O6 Re2 Se2, 0.0365(C1 H2 Cl2)'
_chemical_formula_sum            'C22.0365 H14.073 Cl0.073 N2 O6 Re2 Se2'
_chemical_formula_weight         935.77
_chemical_name_systematic
'hexacarbonylbis(\m-benzeneselenolato)(\m-pyridazine-\kN1:\kN2)dirhenium0.5(dichloromethane solvate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
;
2017-02-22 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6624(8)
_cell_length_b                   18.0556(13)
_cell_length_c                   11.5828(8)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.40
_cell_volume                     2433.0(3)
_computing_structure_refinement
;
SHELX-2014/7: Sheldrick, G. M.
Acta Crystallogr., Sect. C: Struct. Chem. 71, 2015, 3-8.
;
_computing_structure_solution
;
SIR2014: Burla, M. C.; Caliandro, R.; Carrozzini, B.; Cascarano, G. L.;
Cuocci, C.; Giacovazzo, C.; Mallamo, M.; Mazzone, A.; Polidori, G.
J. Appl. Crystallogr. 48, 2015, 306-309.
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.5\% \w steps, collecting
2160 frames each at 15 s exposure keeping the detector at 6.0 cm from the
sample. Intensity decay was monitored by recollecting the initial 50 frames
at the end of data collection and analysing the duplicate reflections.
;
_diffrn_measurement_device_type  'Brucker APEX II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46670
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.607
_diffrn_reflns_theta_min         2.082
_exptl_absorpt_coefficient_mu    12.982
_exptl_absorpt_correction_T_max  0.593
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1: Bruker AXS Inc., Madison, Wisconsin, USA.
Reflections employed for parameter determination: 31565
Maximum odd and even orders for spherical harmonics: 3 and 6
Effective data to parameter ratio: 12.0
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.555
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1710
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane in a dichloromethane
solution at 248 K.
;
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.547
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6433
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0189P)^2^+3.4619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5453
_reflns_number_total             6433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02548c3.cif
_cod_data_source_block           3a
_cod_database_code               7056552
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.343
_shelx_estimated_absorpt_t_max   0.593
_shelx_res_checksum              64478