Triruthenium and Triosmium Carbonyl Cluster Complexes Containing Deprotonated Di(2-pyridyl)amine in Unusual Coordination Modes
Cabeza, Javier A.; del Río, Ignacio; García-Granda, Santiago; Riera, Víctor; Suárez, Marta; Organometallics 21 (2002) 2540–; doi:10.1021/om020073m

data_4076816
_publ_section_title
;
 Triruthenium and Triosmium Carbonyl Cluster Complexes Containing
 Deprotonated Di(2-pyridyl)amine in Unusual Coordination Modes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2540
_journal_paper_doi               10.1021/om020073m
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source
;
 Synthesis. Crystallization from CH~2~Cl~2~/THF/pentane
 at room temperature.
;
_chemical_formula_sum            'C19 H9 N3 O9 Ru3'
_chemical_formula_weight         726.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.09(3)
_cell_angle_beta                 77.17(3)
_cell_angle_gamma                76.71(2)
_cell_formula_units_Z            2
_cell_length_a                   8.575(4)
_cell_length_b                   8.8114(17)
_cell_length_c                   15.479(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      15.3
_cell_volume                     1109.8(6)
_computing_cell_refinement       'CRYSDA (Beurskens et al., 1992)'
_computing_data_reduction        'REFLEX (Garcia-Granda et al., 1999)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w-2\q scan technique'
_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  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4657
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        5.74
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'xabs2 (Parkin et al., 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4349
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.7312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                3620
_reflns_number_total             4349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020073m.cif
_cod_data_source_block           1
_cod_original_cell_volume        1109.9(6)
_cod_database_code               4076816