Cationic 2,6-bis(imino)pyridine iron and cobalt complexes: synthesis, structures, ethylene polymerisation and ethylene/polar monomer co-polymerisation studies
George J. P. Britovsek; Vernon C. Gibson; Stefan K. Spitzmesser; Kilian P. Tellmann; Andrew J. P. White; David J. Williams; J. Chem. Soc., Dalton Trans.  (2002) 1159–1171; doi:10.1039/b106614p

data_7011008
_publ_section_title
;
 Cationic 2,6-bis(imino)pyridine iron and cobalt complexes: synthesis,
 structures, ethylene polymerisation and ethylene/polar monomer
 co-polymerisation studies
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1159
_journal_page_last               1171
_journal_paper_doi               10.1039/b106614p
_journal_year                    2002
_chemical_formula_sum            'C34.5 H50 Cl4 F6 Fe N3 O2 Sb'
_chemical_formula_weight         972.17
_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
_cell_angle_alpha                84.223(15)
_cell_angle_beta                 78.89(2)
_cell_angle_gamma                68.341(15)
_cell_formula_units_Z            2
_cell_length_a                   10.075(2)
_cell_length_b                   13.265(3)
_cell_length_c                   18.925(3)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      5.18
_cell_volume                     2305.4(8)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8617
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        19.40
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.8176
_exptl_absorpt_correction_T_min  0.7358
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       prisms
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.1711
_refine_ls_R_factor_obs          0.0820
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2485
_refine_ls_wR_factor_obs         0.1854
_reflns_number_observed          4073
_reflns_number_total             8112
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106614p.txt
_cod_data_source_block           VG9844
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0931P)^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^)+(0.0931P)^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        2305.4(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.50 H50 N3 O2 Cl4 Fe F6 Sb'
_cod_database_code               7011008