Iridium−Molybdenum Carbido Complex via C−Se Activation of a Selenocarbonyl Ligand: (μ-Se2)[Ir2{C≡Mo(CO)2(Tp*)}2(CO)2(PPh3)2] (Tp* = hydrotris(dimethylpyrazolyl)borate)
Cade, Ian A.; Hill, Anthony F.; McQueen, Caitlin M. A.; Organometallics 28 (2009) 6639–; doi:10.1021/om9008873

data_4070502
_publ_section_title
;
 Iridium&#x2212;Molybdenum Carbido Complex via C&#x2212;Se Activation of a
 Selenocarbonyl Ligand: (\m-Se2)[Ir2{C\\tb Mo(CO)2(Tp*)}2(CO)2(PPh3)2]
 (Tp* = hydrotris(dimethylpyrazolyl)borate)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6639
_journal_paper_doi               10.1021/om9008873
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C74 H74 B2 Ir2 Mo2 N12 O6 P2 Se2'
_chemical_formula_sum            'C74 H74 B2 Ir2 Mo2 N12 O6 P2 Se2'
_chemical_formula_weight         2045.2830
_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
_cell_angle_alpha                110.6570(10)
_cell_angle_beta                 95.2780(10)
_cell_angle_gamma                99.1850(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5985(3)
_cell_length_b                   16.2000(3)
_cell_length_c                   21.0841(4)
_cell_measurement_reflns_used    63220
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.6
_cell_volume                     4546.15(16)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16046
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         2.718
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.073
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;

;
_refine_diff_density_max         2.09
_refine_diff_density_min         -2.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8650
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         15989
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002843
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0750
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0750
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                11755
_reflns_number_total             16046
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.80
_oxford_diffrn_Wilson_scale      52.70
_oxford_refine_ls_r_factor_ref   0.0467
_oxford_refine_ls_scale          0.15530(3)
_oxford_reflns_number_all        15989
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om9008873_si_001.cif
_cod_data_source_block           1
_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_cell_volume        4546.16(16)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4070502