Microwave methods for the synthesis of paddlewheel diruthenium compounds with N,N-donor ligands
Herrero, Santiago; Jiménez-Aparicio, Reyes; Perles, Josefina; Priego, José L.; Saguar, Susana; Urbanos, Francisco A.; Green Chemistry 13 (2011) 1885–; doi:10.1039/c0gc00800a

data_7206165
_publ_section_title
;
 Microwave methods for the synthesis of paddlewheel diruthenium
 compounds with N,N-donor ligands
;
_journal_issue                   7
_journal_name_full               'Green Chemistry'
_journal_page_first              1885
_journal_paper_doi               10.1039/c0gc00800a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C48 H40 N12 Ru2'
_chemical_formula_sum            'C48 H40 N12 Ru2'
_chemical_formula_weight         987.06
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7417(15)
_cell_length_b                   25.884(2)
_cell_length_c                   9.8779(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4791.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1351
_diffrn_reflns_av_sigmaI/netI    0.2077
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45021
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.00(6)
_refine_ls_extinction_coef       0.00003(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         11992
_refine_ls_number_restraints     385
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                4593
_reflns_number_total             11992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0gc00800a.txt
_cod_data_source_block           jru22
_cod_original_cell_volume        4791.8(7)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7206165