<i>tert</i>-Butyl isocyanide-1κ<i>C</i>-di-μ-carbonyl-2:3κ^4^<i>C</i>-nonacarbonyl-1κ^3^<i>C</i>,2κ^3^<i>C</i>,3κ^3^<i>C</i>-<i>triangulo</i>-diironosmium
Tegel, Marcus; Evans, Cameron; Farrugia, Louis J.; Acta Crystallographica Section E 62 (2006) m475–m477; doi:10.1107/S1600536806004235

data_2208346
_publ_section_title
;<i>tert</i>-Butyl
 isocyanide-1\k<i>C</i>-di-\m-carbonyl-2:3\k^4^<i>C</i>-nonacarbonyl-1\k^3^<i>C</i>,2\k^3^<i>C</i>,3\k^3^<i>C</i>-<i>triangulo</i>-diironosmium
;
_journal_coeditor_code           HG6300
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m475
_journal_page_last               m477
_journal_paper_doi               10.1107/S1600536806004235
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe2 Os (C5 H9 N) (C O)11]'
_chemical_formula_moiety         'C16 H9 Fe2 N O11 Os'
_chemical_formula_sum            'C16 H9 Fe2 N O11 Os'
_chemical_formula_weight         693.14
_chemical_name_systematic
;
tert-Butyl isocyanide-1\kC-di-\m-carbonyl-2:3\k^4^C-nonacarbonyl-
1\k^3^C,2\k^3^C,3\k^3^C-triangulo-diironosmium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.8290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6861(2)
_cell_length_b                   11.6142(2)
_cell_length_c                   15.5189(2)
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.2
_cell_volume                     2005.14(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40723
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
 Crystal is twinned about the 1 0 1 real axis with twin matrix
 -0.411  0   0.589
  0     -1   0
 1.411   0   0.411
 The proportion of overlapped second component refines to 0.207(1)
 Data were processed with MakeHKLF5 to give HKLF5.HKL file which was
 used for refinement. 445 reflections most badly affected by the
 twinning were removed (predicted partial overlaps).
 Before twin treatment,  R1 = 0.0609, with delta(rho) in the range
 8.64 -> -3.67 electrons /A-3.
 The range of indices reported refer to the main component.
;
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    7.809
_exptl_absorpt_correction_T_max  0.452
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.23
_refine_ls_extinction_coef       0.00067(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.12
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0019P)^2^+10.979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                4019
_reflns_number_total             4158
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6300.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208346
_cod_database_fobs_code          2208346