High-nuclearity ruthenium carbonyl cluster complexes derived from 2-amino-6-methylpyridine: synthesis of nonanuclear derivatives containing mu4- and mu5-oxo ligands.
Cabeza, Javier A.; del Río, Ignacio; García-Alvarez, Pablo; Miguel, Daniel; Inorganic chemistry 45 (2006) 6020–6027; doi:10.1021/ic060433o

data_4350307
_publ_section_title
;
 High-nuclearity ruthenium carbonyl cluster complexes derived from
 2-amino-6-methylpyridine: synthesis of nonanuclear derivatives containing
 mu4- and mu5-oxo ligands.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6020
_journal_page_last               6027
_journal_paper_doi               10.1021/ic060433o
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~ /
 hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C33 H16 N4 O22 Ru9, C H2 Cl2'
_chemical_formula_sum            'C34 H18 Cl2 N4 O22 Ru9'
_chemical_formula_weight         1815.06
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                86.5770(10)
_cell_angle_beta                 87.1220(10)
_cell_angle_gamma                85.8630(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3849(2)
_cell_length_b                   11.01080(10)
_cell_length_c                   21.9664(3)
_cell_measurement_reflns_used    7654
_cell_measurement_temperature    150(2)
_cell_volume                     2498.10(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16875
_diffrn_reflns_theta_full        70.10
_diffrn_reflns_theta_max         70.10
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    23.092
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.280
_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            black
_exptl_crystal_density_diffrn    2.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00114(5)
_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   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         9221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+5.3009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                8284
_reflns_number_total             9221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060433osi20060314_110736.cif
_cod_data_source_block           4_(pg106b)
_cod_database_code               4350307