Luminescent Hydrido-Carbonyl Clusters of Rhenium Containing Bridging 1,2-Diazine Ligands
Panigati, Monica; Donghi, Daniela; D'Alfonso, Giuseppe; Mercandelli, Pierluigi; Sironi, Angelo; D'Alfonso, Laura; Inorganic Chemistry 45 (2006) 10909–10921; doi:10.1021/ic061467z

data_4333132
_publ_section_title
;
 Luminescent Hydrido-Carbonyl Clusters of Rhenium Containing Bridging
 1,2-Diazine Ligands
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10909
_journal_page_last               10921
_journal_paper_doi               10.1021/ic061467z
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C20 H12 N4 O12 Re4'
_chemical_formula_sum            'C20 H12 N4 O12 Re4'
_chemical_formula_weight         1245.18
_chemical_name_systematic
;
dodecacarbonyltetra-\m-hydrobis(\m-pyridazine-\kN1:\kN2)tetrarhenium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.354(4)
_cell_length_b                   16.312(8)
_cell_length_c                   10.512(5)
_cell_measurement_reflns_used    5257
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.4
_cell_volume                     1354.1(11)
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELX97. Universit\"at G\"ottingen, Germany.
;
_computing_structure_solution
;
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.3\% \w steps, collecting
2400 frames each at 20 s exposure keeping the detector at 4.7 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 SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14161
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    17.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universit\"at G\"ottingen, Germany.
Reflections employed for parameter determination: 13035
Maximum odd and even orders for spherical harmonics: 3 and 6
Effective data to parameter ratio: 4.6
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane
in a tetrahydrofuran solution at 248 K.
;
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0169
_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^)+(0.011P)^2^+4.15P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                2382
_reflns_number_total             2393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic061467zsup1.cif
_cod_data_source_block           squarePYDZ(4a)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4333132