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_4067478
_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            'C36 H50 Au Cl P2 Zr2'
_chemical_formula_weight         959.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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                   11.2225(10)
_cell_length_b                   11.2225(10)
_cell_length_c                   28.170(3)
_cell_measurement_reflns_used    8406
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3547.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- and \f-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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            64727
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.891
_exptl_absorpt_correction_T_max  0.4265
_exptl_absorpt_correction_T_min  0.3557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_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     473
_refine_ls_number_reflns         10720
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                9591
_reflns_number_total             10720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009763_si_001.cif
_cod_data_source_block           susy2
_cod_original_cell_volume        3547.8(6)
_cod_original_sg_symbol_H-M      'P 41 '
_cod_database_code               4067478