Aluminum Alkyl-Mediated Route to NovelN,N,O-Chelates for Five-Coordinate Iron(II) Chloride Complexes: Synthesis, Structures, and Ethylene Polymerization Studies
Gibson, Vernon C.; Redshaw, Carl; Solan, Gregory A.; White, Andrew J. P.; Williams, David J.; Organometallics 26 (2007) 5119–; doi:10.1021/om700611q

data_4073772
_publ_section_title
;
 Aluminum Alkyl-Mediated Route to NovelN,N,O-Chelates for Five-Coordinate
 Iron(II) Chloride Complexes:&#x00A0; Synthesis, Structures, and Ethylene
 Polymerization Studies
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5119
_journal_paper_doi               10.1021/om700611q
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C24 H33 Cl2 Fe N3 O'
_chemical_formula_weight         506.28
_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                 109.22(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.481(2)
_cell_length_b                   12.229(2)
_cell_length_c                   18.486(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.94
_cell_measurement_theta_min      5.15
_cell_volume                     2664.3(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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3662
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        14.67
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.990
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3025
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_obs          0.0698
_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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1690
_refine_ls_wR_factor_obs         0.1278
_reflns_number_observed          1887
_reflns_number_total             3476
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om700611q-file002.cif
_cod_data_source_block           Compound_2a
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0283P)^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^)+(0.0283P)^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        2664.2(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C24 H33 N3 O Cl2 Fe'
_cod_database_code               4073772