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_4084352
_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         'C35 H55 P Zr'
_chemical_formula_sum            'C35 H55 P Zr'
_chemical_formula_weight         598.01
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.306(2)
_cell_length_b                   18.527(5)
_cell_length_c                   21.323(5)
_cell_measurement_reflns_used    14614
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.11
_cell_volume                     3281.3(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17164
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280.00
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.780
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3877 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     375
_refine_ls_number_reflns         9185
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.2636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                8213
_reflns_number_total             9189
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500536c_si_002.cif
_cod_data_source_block           15b_ns147
_cod_depositor_comments
'Adding full bibliography for 4084349--4084356.cif.'
_cod_original_cell_volume        3281.4(14)
_cod_database_code               4084352