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_4076427
_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
'C56 H46 Ir O4 P4 Ru, C F3 O3 S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C57.5 H47 Cl F3 Ir O7 P4 Ru S'
_chemical_formula_weight         1391.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.2753(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.5797(11)
_cell_length_b                   23.6325(15)
_cell_length_c                   26.4280(17)
_cell_measurement_reflns_used    7473
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.18
_cell_volume                     10933.1(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45746
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.975
_exptl_absorpt_correction_T_max  0.7355
_exptl_absorpt_correction_T_min  0.3977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5512
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         12470
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0505P)^2^+12.4433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                10108
_reflns_number_total             12470
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om201201h_si_001.cif
_cod_data_source_block           9-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      'I 2/a'
_cod_database_code               4076427