Iron and Cobalt Ethylene Polymerization Catalysts Bearing 2,6-Bis(Imino)Pyridyl Ligands: Synthesis, Structures, and Polymerization Studies
George J. P. Britovsek; Michael Bruce; Vernon C. Gibson; Brian S. Kimberley; Peter J. Maddox; Sergio Mastroianni; Stuart J. McTavish; Carl Redshaw; Gregory A. Solan; Staffan Strömberg; Andrew J. P. White; David J. Williams; Journal of the American Chemical Society 121 (1999) 8728–8740; doi:10.1021/ja990449w

data_4116542
_publ_section_title
;
 Iron and Cobalt Ethylene Polymerization Catalysts Bearing
 2,6-Bis(Imino)Pyridyl Ligands: Synthesis, Structures, and Polymerization
 Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8728
_journal_page_last               8740
_journal_paper_doi               10.1021/ja990449w
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C29 H34 Br2 Fe N4'
_chemical_formula_weight         654.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.409(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.536(2)
_cell_length_b                   15.273(3)
_cell_length_c                   14.676(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      5.82
_cell_volume                     3012.2(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4663
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.64
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.293
_exptl_absorpt_correction_T_max  0.7345
_exptl_absorpt_correction_T_min  0.2910
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Deep blue'
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00019(4)
_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_all   1.021
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_obs          0.0592
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1451
_refine_ls_wR_factor_obs         0.1180
_reflns_number_observed          2738
_reflns_number_total             4467
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990449w_2.cif
_cod_data_source_block           VG9853
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3012.2(8)
_cod_original_formula_sum        'C29 H34 N4 Br2 Fe'
_cod_database_code               4116542