Synthesis of an Amino-Functionalizedansa-Zirconocene by Intramolecular Photochemical Enamine [2+2]Cycloaddition
Tumay, Tülay Aslı; Kehr, Gerald; Fröhlich, Roland; Erker, Gerhard; Organometallics 28 (2009) 4513–; doi:10.1021/om9003576

data_4069691
_publ_section_title
;
 Synthesis of an Amino-Functionalizedansa-Zirconocene by Intramolecular
 Photochemical Enamine [2+2]Cycloaddition
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4513
_journal_paper_doi               10.1021/om9003576
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C24 H32 Cl2 N2 Zr'
_chemical_formula_weight         510.64
_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                86.038(1)
_cell_angle_beta                 68.639(1)
_cell_angle_gamma                63.421(1)
_cell_formula_units_Z            2
_cell_length_a                   10.5561(2)
_cell_length_b                   10.9379(2)
_cell_length_c                   12.3165(3)
_cell_measurement_reflns_used    1155
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     1176.88(4)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11489
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.9326
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.017(2)
_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   1.035
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+5.1859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                3868
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003576_si_003.cif
_cod_data_source_block           erk4914
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069691