A Rare η2-Butadienyl Complex from an Alkyne Double Insertion with Double Vinylidene Rearrangement
Xingwei Li; Christopher D. Incarvito; Robert H. Crabtree; Journal of the American Chemical Society 125 (2003) 3698–3699; doi:10.1021/ja0297281

data_4113609
_publ_contact_author
;
     Dr. Robert H. Crabtree
     Department of Chemistry
     Yale University
     225 Prospect St
     New Haven, CT 06520-8107
     USA
;
_publ_contact_author_email       robert.crabtree@yale.edu
_publ_contact_author_fax         '+203 432 6144'
_publ_contact_author_phone       '+203 432 3925'
_publ_section_title
;
 A Rare \h2-Butadienyl Complex from an Alkyne Double Insertion with Double
 Vinylidene Rearrangement
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3698
_journal_page_last               3699
_journal_paper_doi               10.1021/ja0297281
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C62 H52 F6 Ir O P2 Sb'
_chemical_formula_weight         1302.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.22(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.486(3)
_cell_length_b                   15.669(3)
_cell_length_c                   27.495(6)
_cell_measurement_temperature    296(2)
_cell_volume                     5365(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20065
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.104
_exptl_absorpt_correction_T_max  0.5108
_exptl_absorpt_correction_T_min  0.5108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         10520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                6526
_reflns_number_total             10520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0297281si20030208_050933_1.cif
_cod_data_source_block           xl04
_cod_original_cell_volume        5364.3(19)
_cod_database_code               4113609