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_4063869
_publ_section_title
;
 Alkyne/Methylene Coupling at Adjacent Iridium/Osmium Centers: Facile
 Carbon&#x2212;Carbon and Carbon&#x2212;Oxygen Bond Formation
;
_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         'C61 H54 Ir O7 Os P4, B F4'
_chemical_formula_sum            'C61 H54 B F4 Ir O7 Os P4'
_chemical_formula_weight         1492.13
_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                97.5953(7)
_cell_angle_beta                 90.3465(7)
_cell_angle_gamma                111.6572(7)
_cell_formula_units_Z            2
_cell_length_a                   11.3495(7)
_cell_length_b                   13.8540(9)
_cell_length_c                   19.5589(12)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.20
_cell_volume                     2828.2(3)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24859
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    4.774
_exptl_absorpt_correction_T_max  0.6074
_exptl_absorpt_correction_T_min  0.1476
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         6.753
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         12821
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+10.1474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                11661
_reflns_number_total             12821
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1009999_si_002.cif
_cod_data_source_block           8-BF4
_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               4063869