High-Nuclearity Osmium Carbonyl Cluster Complexes Containing (6-Methylpyrid-2-yl)imido Ligands. Synthesis of Hepta-, Octa-, and Nonanuclear Derivatives
Cabeza, Javier A.; del Río, Ignacio; García-Álvarez, Pablo; Miguel, Daniel; Organometallics 26 (2007) 3212–; doi:10.1021/om070201c

data_4073263
_publ_section_title
;
 High-Nuclearity Osmium Carbonyl Cluster Complexes Containing
 (6-Methylpyrid-2-yl)imido Ligands. Synthesis of Hepta-, Octa-, and
 Nonanuclear Derivatives
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3212
_journal_paper_doi               10.1021/om070201c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C30 H12 N4 O19 Os9, C H2 Cl2'
_chemical_formula_sum            'C31 H14 Cl2 N4 O19 Os9'
_chemical_formula_weight         2529.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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                97.207(8)
_cell_angle_beta                 93.225(8)
_cell_angle_gamma                91.379(8)
_cell_formula_units_Z            2
_cell_length_a                   10.383(4)
_cell_length_b                   11.184(5)
_cell_length_c                   20.070(8)
_cell_measurement_temperature    296(2)
_cell_volume                     2307.4(16)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10331
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    24.860
_exptl_absorpt_correction_T_max  0.085
_exptl_absorpt_correction_T_min  0.065
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.003
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_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6559
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_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+32.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                5548
_reflns_number_total             6559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070201c-file001.cif
_cod_data_source_block           3_(pg120fdm)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2307.4(17)
_cod_database_code               4073263