Formation of cyclooctatetraenes from zirconacyclopentadienes
Takahashi, Tamotsu; Sun, Wen-Hua; Nakajima, Kiyohiko; Chemical Communications  (1999) 1595–; doi:10.1039/a902788b

data_7125460
_publ_contact_author
;
     Prof. Tamotsu Takahashi
     Catalysis Research Center and Graduate School of Pharmaceutical Sciences
     Hokkaido University
     Kita-ku
     Sapporo 060-0811
     Japan
;
_publ_section_title
;
 Formation of cyclooctatetraenes from zirconacyclopentadienes
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1595
_journal_paper_doi               10.1039/a902788b
_journal_year                    1999
_chemical_compound_source        'local laboratory'
_chemical_formula_analytical     'C32 H56'
_chemical_formula_moiety         'C32 H56'
_chemical_formula_structural     'C32 H56'
_chemical_formula_sum            'C32 H56'
_chemical_formula_weight         440.80
_chemical_name_common            Octapropylcyclooctatetraene
_chemical_name_systematic
;
1,2,3,4,5,6,7,8-Octapropyl-1,3,5,7-cyclooctatetraene
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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   vecmap
_audit_creation_date             99-03-18
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record
;
99-04-16 text and data added by Kiyohiko Nakajima
;
_cell_angle_alpha                88.553(4)
_cell_angle_beta                 83.021(3)
_cell_angle_gamma                87.903(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5552(2)
_cell_length_b                   9.5131(3)
_cell_length_c                   17.1505(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      84.37
_cell_measurement_theta_min      44.23
_cell_volume                     1546.05(10)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1989)'
_computing_data_reduction        xtal_DIFDAT_ADDREF_SORTRF
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    'SHELXS-86 (Sheldric, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Enraf-Nonius CAD4 4-circle-diffractometer'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_detector       scintillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf-Nonius tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .025
_diffrn_reflns_av_sigmaI/netI    .094
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6676
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         74.3
_diffrn_reflns_theta_min         4.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .35
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    .947
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_preparation       'mounted on a glass fibre with epoxy resine'
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         .188
_refine_diff_density_min         -.198
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.64
_refine_ls_goodness_of_fit_obs   2.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     513
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .104
_refine_ls_R_factor_obs          .053
_refine_ls_shift/esd_max         .269
_refine_ls_shift/esd_mean        .032
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w= 1/(\s^2^(F)+0.000225F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .072
_refine_ls_wR_factor_obs         .063
_reflns_d_resolution_high        .801
_reflns_d_resolution_low         9.487
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_observed          3160
_reflns_number_total             6283
_reflns_observed_criterion       refl_observed_if_F~o~_>_3.00_sigma(F~o~)
_cod_data_source_file            902788b.txt
_cod_data_source_block           cytet
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc w=
1/(\s^2^(F)+0.000225F^2^)' was changed to 'calc'. A new data item
'_refine_ls_weighting_details' was created with the value set to 'w=
1/(\s^2^(F)+0.000225F^2^)'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1546.0(1)
_cod_original_sg_symbol_Hall     -P_1
_cod_original_sg_symbol_H-M      P1-
_cod_database_code               7125460