Haptotropic Shift of [5]Cumulenes in Zirconocene Complexes and Effects of Steric Factors
Suzuki, Noriyuki; Yoshitani, Takao; Inoue, Shota; Hashizume, Daisuke; Yoshida, Hajime; Tezuka, Meguru; Ida, Keisuke; Nagashima, Sayoko; Chihara, Teiji; Kobayashi, Osamu; Nanbu, Shinkoh; Masuyama, Yoshiro; Organometallics 33 (2014) 5220–; doi:10.1021/om500536c

data_4084355
_publ_section_title
;
 Haptotropic Shift of [5]Cumulenes in Zirconocene Complexes and Effects of
 Steric Factors
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5220
_journal_paper_doi               10.1021/om500536c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C42 H64 N2 Zr'
_chemical_formula_sum            'C42 H64 N2 Zr'
_chemical_formula_weight         688.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                110.75(4)
_cell_angle_beta                 96.16(4)
_cell_angle_gamma                96.57(5)
_cell_formula_units_Z            4
_cell_length_a                   8.161(3)
_cell_length_b                   22.558(6)
_cell_length_c                   23.013(4)
_cell_measurement_reflns_used    407
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.08
_cell_volume                     3886(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.698
_diffrn_measured_fraction_theta_max 0.698
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20664
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, ????)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.960
_refine_diff_density_min         -2.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     866
_refine_ls_number_reflns         10538
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1144
_refine_ls_shift/su_max          1.419
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3549
_reflns_number_gt                7846
_reflns_number_total             10538
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500536c_si_002.cif
_cod_data_source_block           16_Zr-M
_cod_depositor_comments
'Adding full bibliography for 4084349--4084356.cif.'
_cod_original_cell_volume        3885(3)
_cod_database_code               4084355