Synthesis, Characterization and Reactivity of Group 4 Metallocene Bis(diphenylphosphino)acetylene Complexes-A Reactivity and Bonding Study
Martin Haehnel; Sven Hansen; Kathleen Schubert; Perdita Arndt; Anke Spannenberg; Haijun Jiao; Uwe Rosenthal; Journal of the American Chemical Society 135 (2013) 17556–17565; doi:10.1021/ja409320k

data_4121173
_publ_section_title
;
 Synthesis, Characterization and Reactivity of Group 4 Metallocene
 Bis(diphenylphosphino)acetylene Complexes-A Reactivity and Bonding Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17556
_journal_page_last               17565
_journal_paper_doi               10.1021/ja409320k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C95.8 H87.2 P4 Zr2'
_chemical_formula_weight         1544.78
_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                78.3890(10)
_cell_angle_beta                 68.9040(10)
_cell_angle_gamma                79.2090(10)
_cell_formula_units_Z            2
_cell_length_a                   15.5727(4)
_cell_length_b                   15.8919(4)
_cell_length_c                   16.9596(4)
_cell_measurement_reflns_used    9346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.22
_cell_volume                     3805.35(17)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            119043
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         17446
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0502P)^2^+5.8156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                14773
_reflns_number_total             17446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409320k_si_005.cif
_cod_data_source_block           ax0219
_cod_original_cell_volume        3805.35(16)
_cod_original_formula_sum        'C95.80 H87.20 P4 Zr2'
_cod_database_code               4121173