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_4076425
_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
'C57 H48 Ir O4 P4 Ru, C F3 O3 S, 0.5(C H2 Cl2), C4 H10 O'
_chemical_formula_sum            'C62.5 H59 Cl F3 Ir O8 P4 Ru S'
_chemical_formula_weight         1479.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 96.598(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.714(3)
_cell_length_b                   17.3092(14)
_cell_length_c                   20.5712(17)
_cell_measurement_reflns_used    5502
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.246
_cell_measurement_theta_min      2.434
_cell_volume                     12278.8(18)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46539
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  0.6915
_exptl_absorpt_correction_T_min  0.4837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5912
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 Attempts to refine peaks of residual electron density as partially
 occupied/disordered solvent dichloromethane and diethylether molecules
 were unsuccessful. The data were corrected for disordered electron
 density through use of the SQUEEZE procedure as implemented in PLATON.
 A total solvent accessible void volume of 1885.2 A3 and electron count
 of 685.4 electons were found, consistent with an additional 1
 equivalent of diethylether and 0.5 equivalents of dichloromethane
 molecules per asymmetic unit.
;
_refine_diff_density_max         1.849
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12566
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0645P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                8816
_reflns_number_total             12566
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om201201h_si_001.cif
_cod_data_source_block           2-CF3SO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_H-M      'C 2/c'
_cod_database_code               4076425