Approaches to Triosmium Carbonyl Cluster Compounds Derived from Benzophenone Imine. Characterization of Terminal Imino, Bridging Amido, and Orthometalated Imino Derivatives
Cabeza, Javier A.; del Río, Ignacio; Grepioni, Fabrizia; Riera, Víctor; Organometallics 19 (2000) 4643–; doi:10.1021/om0004139

data_4077539
_publ_section_title
;
 Approaches to Triosmium Carbonyl Cluster Compounds Derived from
 Benzophenone Imine. Characterization of Terminal Imino, Bridging Amido,
 and Orthometalated Imino Derivatives
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4643
_journal_paper_doi               10.1021/om0004139
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C41 H28 N2 O9 Os3'
_chemical_formula_weight         1263.25
_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                101.681(4)
_cell_angle_beta                 106.035(3)
_cell_angle_gamma                94.080(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0290(10)
_cell_length_b                   12.2780(10)
_cell_length_c                   15.922(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2010.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0762
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24718
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    9.511
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  .23
_exptl_absorpt_correction_type   'Bruker area detector'
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.00000(6)
_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   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         11680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                5443
_reflns_number_total             11680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0004139.cif
_cod_data_source_block           3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077539