Formation and Structural and Dynamic Features of Atropisomeric η2-Iminoacyl Zirconium Complexes
Spies, Patrick; Kehr, Gerald; Kehr, Seda; Fröhlich, Roland; Erker, Gerhard; Organometallics 26 (2007) 5612–; doi:10.1021/om7005968

data_4073741
_publ_section_title
;
 Formation and Structural and Dynamic Features of Atropisomeric
 \h2-Iminoacyl Zirconium Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5612
_journal_paper_doi               10.1021/om7005968
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C46.5 H43 Cl N P Zr'
_chemical_formula_weight         773.46
_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                81.52(1)
_cell_angle_beta                 79.70(1)
_cell_angle_gamma                71.34(1)
_cell_formula_units_Z            2
_cell_length_a                   8.412(1)
_cell_length_b                   11.119(1)
_cell_length_c                   22.698(1)
_cell_measurement_reflns_used    5442
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     1969.7(3)
_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      198(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonisu FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20218
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.8334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0523P)^2^+0.9773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                8218
_reflns_number_total             9348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7005968-file002.cif
_cod_data_source_block           erk3566(13a)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46.50 H43 Cl N P Zr'
_cod_database_code               4073741