Iminopyridine Complexes of 3d Metals for Ethylene Polymerization: Comparative Structural Studies and Ligand Size Controlled Chain Termination
Kaul, Franz A. R.; Puchta, Gerd T.; Frey, Guido D.; Herdtweck, Eberhardt; Herrmann, Wolfgang A.; Organometallics 26 (2007) 988–; doi:10.1021/om060857q

data_4072591
_publ_section_title
;
 Iminopyridine Complexes of 3d Metals for Ethylene Polymerization:&#x00A0;
 Comparative Structural Studies and Ligand Size Controlled Chain
 Termination
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              988
_journal_paper_doi               10.1021/om060857q
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        ' see text '
_chemical_formula_moiety         'C33 H27 Cl2 Fe N3'
_chemical_formula_sum            'C33 H27 Cl2 Fe N3'
_chemical_formula_weight         592.33
_chemical_name_systematic
;
 not known
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.136(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6461(3)
_cell_length_b                   16.1220(2)
_cell_length_c                   15.8418(3)
_cell_measurement_reflns_used    43241
_cell_measurement_temperature    143(1)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.33
_cell_volume                     3132.03(10)
_computing_cell_refinement       'DENZO (Nonius, 1998b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 1998a)'
_computing_data_reduction        'DENZO (Nonius, 1998b)'
_computing_molecular_graphics    'PLATON (Spek, 2006)'
_computing_publication_material  'PLATON (Spek, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      143(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12033
_diffrn_reflns_reduction_process
;
 with the Kappa CCD software Scale-Pack 
;
_diffrn_reflns_theta_full        26.20
_diffrn_reflns_theta_max         26.20
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Denzo-SNM; Scale-Pack
;
_exptl_crystal_colour            ' blue '
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0318P)^2^+1.4244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                5303
_reflns_number_total             6247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060857qsi20060919_050002.cif
_cod_data_source_block           KAUB-4024-143
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3132.0(1)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072591