Synthesis and Structure of 1-Zirconacyclopent-3-yne Complexes without Substituents Adjacent to the Triple Bond
Noriyuki Suzuki; Naoto Aihara; Hidemichi Takahara; Takaaki Watanabe; Masakazu Iwasaki; Masahiko Saburi; Daisuke Hashizume; Teiji Chihara; Journal of the American Chemical Society 126 (2004) 60–61; doi:10.1021/ja0385742

data_4060213
_publ_contact_author_address
;
    Chemical Analysisi Division, RIKEN, Wako, Saitama, 351-0198, Japan
;
_publ_contact_author_email       ' nsuzuki@postman.riken.go.jp'
_publ_contact_author_fax         ' +81-48-462-4631 '
_publ_contact_author_name        ' Noriyuki Suzuki'
_publ_section_title
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Synthesis and Structure of 1-Zirconacyclopent-3-yne Complexes without
Substituents Adjacent to the Triple Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              60
_journal_page_last               61
_journal_paper_doi               10.1021/ja0385742
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C22 H30 Zr'
_chemical_formula_weight         385.68
_chemical_name_systematic
;
 Cp2Zr(mu:hapto-2:hapto2-1,2,3-butatriene)Zr(PMe3)Cp2 6
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 91.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.7687(11)
_cell_length_b                   8.7564(3)
_cell_length_c                   8.0887(4)
_cell_measurement_reflns_used    38106
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.52
_cell_volume                     1895.64(14)
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10
_diffrn_measurement_device_type  'Rigaku Raxis CS'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       -12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38106
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.7228
_exptl_absorpt_correction_T_min  0.5380
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rock
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.60
_refine_ls_extinction_coef       0.0083(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+1.6122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                4732
_reflns_number_total             5414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+1.6122P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+1.6122P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060213