Synthesis and Reactivity of Bis(η5:η1-pentafulvene)zirconium Complexes
Ebert, Hanna; Timmermann, Vanessa; Oswald, Tim; Saak, Wolfgang; Schmidtmann, Marc; Friedemann, Marion; Haase, Detlev; Beckhaus, Rüdiger; Organometallics 33 (2014) 1440–; doi:10.1021/om500031s

data_4082768
_publ_section_title
;
 Synthesis and Reactivity of Bis(\h5:\h1-pentafulvene)zirconium Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1440
_journal_paper_doi               10.1021/om500031s
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C135 H149 O3 Zr3'
_chemical_formula_weight         2093.20
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.7190(10)
_cell_angle_beta                 74.7090(10)
_cell_angle_gamma                73.9880(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8072(4)
_cell_length_b                   15.4266(4)
_cell_length_c                   25.8025(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.28
_cell_volume                     5463.9(2)
_computing_cell_refinement       'Bruker AXS SAINT V8.27B'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker AXS SAINT V8.27B'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            118642
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.8935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2206
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1324
_refine_ls_number_reflns         28214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                19393
_reflns_number_total             28214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500031s_si_001.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082768