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_4063870
_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         'C59 H50 Ir O7 Os P4, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C61 H54 B Cl4 F4 Ir O7 Os P4'
_chemical_formula_weight         1633.93
_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                87.307(13)
_cell_angle_beta                 76.756(13)
_cell_angle_gamma                84.880(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5146(14)
_cell_length_b                   14.703(2)
_cell_length_c                   19.180(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      11.96
_cell_measurement_theta_min      10.19
_cell_volume                     3147.0(8)
_computing_cell_refinement       'Enraf-Nonius CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'Enraf-Nonius CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 2008)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\q-2\q 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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11386
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    4.463
_exptl_absorpt_correction_T_max  0.5738
_exptl_absorpt_correction_T_min  0.1716
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 2008)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.732
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         11013
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0458
_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^)+(0.1052P)^2^+2.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                8501
_reflns_number_total             11013
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1009999_si_002.cif
_cod_data_source_block           12-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 
;
_cod_database_code               4063870