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_4113610
_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
_chemical_name_systematic
; 
 ? 
;
_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                 90.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.507(3)
_cell_length_b                   18.091(4)
_cell_length_c                   20.457(4)
_cell_measurement_temperature    296(2)
_cell_volume                     5368.7(19)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21686
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    3.101
_exptl_absorpt_correction_T_max  0.4564
_exptl_absorpt_correction_T_min  0.4564
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       Block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.438
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         12712
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                8739
_reflns_number_total             12712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0297281si20030208_050933_2.cif
_cod_data_source_block           xl02
_cod_database_code               4113610