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_4076817
_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
;
 Suitable crystals were obtained by slow evaporation of a diethyl ether
solution of the compound at room temperature
;
_chemical_formula_sum            'C20 H9 N3 O10 Os3'
_chemical_formula_weight         1021.90
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.81(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.595(8)
_cell_length_b                   25.075(5)
_cell_length_c                   12.795(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      8.2
_cell_volume                     4930(5)
_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    'DIRDIF96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10018
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        10.11
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.483
_exptl_absorpt_correction_T_max  0.134
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'xabs2 (Parkin et al., 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.181
_refine_diff_density_min         -2.409
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                5648
_reflns_number_total             9657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020073m.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4076817