Metallic Dysprosium Induced Silyl Radical Reactions: Intermolecular Cyclization and Reduction of Alkynes and Imines
Zhu, Zhenyu; Wang, Jialiang; Zhang, Zhengxing; Xiang, Xu; Zhou, Xigeng; Organometallics 26 (2007) 2499–; doi:10.1021/om070148s

data_4073185
_publ_section_title
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 Metallic Dysprosium Induced Silyl Radical Reactions:&#x00A0;
 Intermolecular Cyclization and Reduction of Alkynes and Imines
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2499
_journal_paper_doi               10.1021/om070148s
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C26 H20 F2 N2'
_chemical_formula_weight         398.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.425(7)
_cell_angle_beta                 95.667(9)
_cell_angle_gamma                90.000(9)
_cell_formula_units_Z            4
_cell_length_a                   8.307(6)
_cell_length_b                   13.991(9)
_cell_length_c                   20.044(13)
_cell_measurement_reflns_used    821
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.635
_cell_measurement_theta_min      2.970
_cell_volume                     2171(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        5.08
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.2401
_refine_ls_R_factor_gt           0.1340
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+4.5351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3184
_refine_ls_wR_factor_ref         0.3932
_reflns_number_gt                3290
_reflns_number_total             7428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070148s-file001.cif
_cod_data_source_block           f60908b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2171(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073185