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_4350310
_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 toluene/
hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C38 H20 N6 O22 Ru9, 0.25(C7 H8)'
_chemical_formula_sum            'C39.75 H22 N6 O22 Ru9'
_chemical_formula_weight         1845.27
_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                94.583(10)
_cell_angle_beta                 97.112(9)
_cell_angle_gamma                94.107(9)
_cell_formula_units_Z            2
_cell_length_a                   11.049(5)
_cell_length_b                   14.805(7)
_cell_length_c                   17.931(9)
_cell_measurement_temperature    296(2)
_cell_volume                     2891(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12695
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. SADABS, Empirical Absorption 
Correction Program; University of Gottingen, 
Gottingen, Germany, 1997.
;
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1749
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         8142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0626
_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
 [1.00000+-1.00000exp(-19.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+62.3694*P+(0.0751P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                6422
_reflns_number_total             8142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060433osi20060314_110736.cif
_cod_data_source_block           7_(pg106mm)
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350310