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_7011012
_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            'C48 H54 F6 Fe N3 O2 Sb'
_chemical_formula_weight         996.54
_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                 90.439(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4639(12)
_cell_length_b                   17.1447(5)
_cell_length_c                   21.5722(12)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      21.63
_cell_volume                     4609.6(5)
_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      193(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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7141
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         3.29
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.720
_exptl_absorpt_correction_T_max  0.5676
_exptl_absorpt_correction_T_min  0.3561
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00026(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   1.033
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         6401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.6099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1270
_refine_ls_wR_factor_obs         0.1157
_reflns_number_observed          5456
_reflns_number_total             6786
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106614p.txt
_cod_data_source_block           VG0005
_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_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^)+(0.0709P)^2^+3.6099P] 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^)+(0.0709P)^2^+3.6099P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C48 H54 N3 O2 Fe Sb F6'
_cod_database_code               7011012