Ambiphilic Reactivity of a Phosphane-Functionalized Cycloheptatrienyl−Cyclopentadienyl Zirconium Sandwich Complex
Büschel, Susanne; Daniliuc, Constantin; Jones, Peter G.; Tamm, Matthias; Organometallics 29 (2010) 671–; doi:10.1021/om9009763

data_4067480
_publ_section_title
;
 Ambiphilic Reactivity of a Phosphane-Functionalized
 Cycloheptatrienyl&#x2212;Cyclopentadienyl Zirconium Sandwich Complex
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              671
_journal_paper_doi               10.1021/om9009763
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C39 H50 O3 P2 W Zr2'
_chemical_formula_weight         995.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.885(2)
_cell_angle_beta                 107.504(2)
_cell_angle_gamma                110.107(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8096(3)
_cell_length_b                   11.7868(2)
_cell_length_c                   16.4711(3)
_cell_measurement_reflns_used    27703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.6196
_cell_measurement_theta_min      2.0569
_cell_volume                     1837.31(8)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_computing_data_collection
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_computing_molecular_graphics    'BRUKER XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56606
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    3.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment
;
The hydrogens of the five- and seven-membered rings were refined freely. 
The hydrogens of the methyl groups were refined using a rigid groups, 
other H atoms were included using a riding model.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         11227
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0326
_reflns_number_gt                9381
_reflns_number_total             11227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009763_si_001.cif
_cod_data_source_block           susy42
_cod_original_cell_volume        1837.31(7)
_cod_database_code               4067480