Activation of a Nonstrained C(sp2)−C(sp2) Single Bond in a Vaska Complex Analogue Using Chelating Assistance
Obenhuber, Andreas; Ruhland, Klaus; Organometallics 30 (2011) 171–; doi:10.1021/om100985r

data_4063847
_publ_section_title
;
 Activation of a Nonstrained C(sp2)&#x2212;C(sp2) Single Bond in a Vaska
 Complex Analogue Using Chelating Assistance
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              171
_journal_paper_doi               10.1021/om100985r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C25 H36 Cl Ir O3 P2'
_chemical_formula_weight         674.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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                   11.3349(3)
_cell_length_b                   14.7840(4)
_cell_length_c                   15.3145(4)
_cell_measurement_reflns_used    2334
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.63
_cell_volume                     2566.33(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Oxford-Diffraction Xcalibur3 '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0228
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37366
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.456
_exptl_absorpt_correction_T_max  0.4949
_exptl_absorpt_correction_T_min  0.2309
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.639
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.527
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+20.2115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                2069
_reflns_number_total             2334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100985r_si_002.cif
_cod_data_source_block           6_3
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4063847