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_4333129
_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         'C36 H22 N6 O12 Re4, 3(C H2 Cl2)'
_chemical_formula_sum            'C39 H28 Cl6 N6 O12 Re4'
_chemical_formula_weight         1730.17
_chemical_name_systematic
;
dodecacarbonyltetra-\m-hydrido(\m-phthalazine-\kN2:\kN3)bis(phthalazine-
\kN2)tetrarhenium dichloromethane solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 128.62(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.445(5)
_cell_length_b                   13.365(2)
_cell_length_c                   24.569(3)
_cell_measurement_reflns_used    15536
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.2
_cell_volume                     9863(4)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
More than a hemisphere of reciprocal space was scanned by 0.3\% \w steps,
collecting 1650 frames each at 40 s exposure keeping the detector at 3.0 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 SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43710
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        10
_exptl_absorpt_coefficient_mu    10.175
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universit\"at G\"ottingen, Germany.
Reflections employed for parameter determination: 28997
Maximum odd and even orders for spherical harmonics: 1 and 4
Effective data to parameter ratio: 13.0
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6416
_exptl_crystal_preparation
;
A sample of [Re~4~(\m~3~-H)~4~(CO)~12~] dissolved in dichloromethane
was treated at room temperature with 2 equivalents of phthalazine.
The mixture was left at room temperature overnight. Crystals were isolated
by filtration.
;
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8704
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0256
_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^)+(0.03P)^2^+1.9P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                6699
_reflns_number_total             8704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic061467zsup1.cif
_cod_data_source_block           spikedPHAL(2b)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4333129