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_4067481
_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            'C18 H25 P Se Zr'
_chemical_formula_weight         442.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.074(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0011(2)
_cell_length_b                   12.1287(4)
_cell_length_c                   14.5060(4)
_cell_measurement_reflns_used    17118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2140
_cell_measurement_theta_min      2.2024
_cell_volume                     1720.66(8)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, 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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61155
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment
;
The hydrogen coordinates of the five- and seven-membered rings were 
refined freely, but the U values were fixed because otherwise several
became negative. 
The hydrogens of the methyl groups were refined using rigid groups; 
other H atoms were included using a riding model.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                6270
_reflns_number_total             8136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009763_si_001.cif
_cod_data_source_block           susy46
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4067481