Characterization of theEIsomer of Tetrasubstituted [5]Cumulene and Trapping of theZIsomer as a Zirconocene Complex
Suzuki, Noriyuki; Ohara, Nozomu; Nishimura, Kosuke; Sakaguchi, Yoshio; Nanbu, Shinkoh; Fukui, Sohei; Nagao, Hirotaka; Masuyama, Yoshiro; Organometallics 30 (2011) 3544–; doi:10.1021/om2002427

data_4064647
_publ_section_title
;
 Characterization of theEIsomer of Tetrasubstituted [5]Cumulene and
 Trapping of theZIsomer as a Zirconocene Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3544
_journal_paper_doi               10.1021/om2002427
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C36 H38 Zr'
_chemical_formula_sum            'C36 H38 Zr'
_chemical_formula_weight         561.92
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            8
_cell_length_a                   52.948(16)
_cell_length_b                   12.536(4)
_cell_length_c                   8.677(3)
_cell_measurement_reflns_used    4638
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      3.08
_cell_volume                     5759(3)
_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    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0472
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -73
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5935
_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  0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2352.00
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.210
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  843 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_coef       0.00001(15)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3046
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                2553
_reflns_number_total             3046
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om2002427_si_004.cif
_cod_data_source_block           '_ns156'
_cod_database_code               4064647