Carbon−Carbon Bond Formation of α-Alkynylzirconacyclopentenes via Cyclization or a Cu/Pd-Mediated Cyclization/Cross-Coupling Sequence with Aryl Iodides
Chen, Jingjin; Li, Yuxue; Gao, Hongjun; Liu, Yuanhong; Organometallics 27 (2008) 5619–; doi:10.1021/om8005245

data_4072020
_publ_section_title
;
 Carbon&#x2212;Carbon Bond Formation of \a-Alkynylzirconacyclopentenes via
 Cyclization or a Cu/Pd-Mediated Cyclization/Cross-Coupling Sequence with
 Aryl Iodides
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5619
_journal_paper_doi               10.1021/om8005245
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H30 N2'
_chemical_formula_weight         442.58
_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                80.274(5)
_cell_angle_beta                 80.161(5)
_cell_angle_gamma                78.185(5)
_cell_formula_units_Z            2
_cell_length_a                   7.961(2)
_cell_length_b                   11.374(3)
_cell_length_c                   14.410(3)
_cell_measurement_reflns_used    782
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.117
_cell_measurement_theta_min      4.367
_cell_volume                     1246.2(5)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.1595
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6526
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0039(12)
_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   0.669
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.669
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                1697
_reflns_number_total             4564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8005245_si_002.cif
_cod_data_source_block           cd27260
_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        1246.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072020