Geminal Carbon‒Hydrogen Bond Activation in Cumulenes Promoted by Adjacent Iridium/Ruthenium Centers
MacDougall, Tiffany J.; Samant, Rahul G.; Trepanier, Steven J.; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 31 (2012) 1857–; doi:10.1021/om201201h

data_4076426
_publ_section_title
;
 Geminal Carbon--Hydrogen Bond Activation in Cumulenes Promoted by
 Adjacent Iridium/Ruthenium Centers
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1857
_journal_paper_doi               10.1021/om201201h
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety
'C59 H50 Ir O4 P4 Ru, C F3 O3 S, 3.5(C4 H8 O)'
_chemical_formula_sum            'C74 H78 F3 Ir O10.5 P4 Ru S'
_chemical_formula_weight         1641.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5564(13)
_cell_length_b                   15.2146(10)
_cell_length_c                   24.4022(16)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.40
_cell_volume                     6889.4(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58677
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.5462
_exptl_absorpt_correction_T_min  0.4237
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.29
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent pentane or tetrahydrofuran carbon or oxygen atoms 
were unsuccessful.  The data were corrected for disordered electron density 
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta 
Crystallogr. 1990, A46, 194&#x0096;201) as implemented in PLATON (Spek, A. L. Acta 
Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 7&#x0096;13.  
PLATON - a multipurpose crystallographic tool.  Utrecht University, 
Utrecht, The Netherlands).  A total solvent-accessible void volume of 1715.9 
angstroms3 with a total electron count of 566 (consistent with 14 molecules 
of solvent tetrahydrofuran, or 3.5 molecules per formula unit of the IrRu 
complex) was found in the unit cell.
;
_refine_diff_density_max         2.007
_refine_diff_density_min         -3.122
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0338P)^2^+42.5779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                7294
_reflns_number_total             8238
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om201201h_si_001.cif
_cod_data_source_block           4-CF3SO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_original_sg_symbol_Hall     '- P 2ac 2n'
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C74 H78 F3 Ir O10.50 P4 Ru S'
_cod_database_code               4076426