Alkyne/Methylene Coupling at Adjacent Iridium/Osmium Centers: Facile Carbon−Carbon and Carbon−Oxygen Bond Formation
MacDougall, Tiffany J.; Llamazares, Angela; Kuhnert, Oliver; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 30 (2011) 952–; doi:10.1021/om1009999

data_4063867
_publ_section_title
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 Alkyne/Methylene Coupling at Adjacent Iridium/Osmium Centers: Facile
 Carbon&#x2212;Carbon and Carbon&#x2212;Oxygen Bond Formation
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              952
_journal_paper_doi               10.1021/om1009999
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C55 H46 Ir O4 Os P4, C F3 O3 S, 3.5(C2 H3 N)'
_chemical_formula_sum            'C63 H56.5 F3 Ir N3.5 O7 Os P4 S'
_chemical_formula_weight         1569.96
_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                91.0983(3)
_cell_angle_beta                 99.1756(3)
_cell_angle_gamma                91.4100(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2757(4)
_cell_length_b                   13.0139(4)
_cell_length_c                   21.2552(7)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.20
_cell_volume                     3077.32(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0104
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27615
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    4.425
_exptl_absorpt_correction_T_max  0.3408
_exptl_absorpt_correction_T_min  0.2233
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         14048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+3.2425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                13394
_reflns_number_total             14048
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1009999_si_002.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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               4063867