Triruthenium and Triosmium Carbonyl Cluster Complexes Containing Bridging Ligands Derived from 2-Amino-7,8-benzoquinoline
Cabeza, Javier A.; del Río, Ignacio; García-Granda, Santiago; Riera, Víctor; Suárez, Marta; Organometallics 21 (2002) 5055–; doi:10.1021/om0205647

data_4077080
_publ_section_title
;
 Triruthenium and Triosmium Carbonyl Cluster Complexes Containing Bridging
 Ligands Derived from 2-Amino-7,8-benzoquinoline
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5055
_journal_paper_doi               10.1021/om0205647
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~/acetone/
hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C22 H8 N2 O9 Ru3'
_chemical_formula_sum            'C22 H8 N2 O9 Ru3'
_chemical_formula_weight         747.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.012(6)
_cell_length_b                   16.902(7)
_cell_length_c                   17.920(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.79
_cell_measurement_theta_min      14.08
_cell_volume                     4721(3)
_computing_cell_refinement       'CRYSDA (Beurskens et al., 1996)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9985
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        3.87
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         9254
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                5010
_reflns_number_total             9254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205647.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077080
_exptl_absorpt_factor_mur        0.293
_exptl_absorpt_correction_t_ave  0.7501
_exptl_absorpt_rmerge_before     0.1237
_exptl_absorpt_rmerge_after      0.1234