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_4350308
_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         'C39 H20 N6 O23 Ru9'
_chemical_formula_sum            'C39 H20 N6 O23 Ru9'
_chemical_formula_weight         1850.24
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 106.252(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.632(7)
_cell_length_b                   14.108(6)
_cell_length_c                   24.727(11)
_cell_measurement_temperature    296(2)
_cell_volume                     5235(4)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22670
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.391
_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    2.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00089(8)
_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   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         7509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0468
_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(-5.70(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+68.4038*P+(0.0065P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                6133
_reflns_number_total             7509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060433osi20060314_110736.cif
_cod_data_source_block           5_(pg106am)
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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      P2(1)/c
_cod_database_code               4350308