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_4073771
_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            'C28 H45.5 Al2 N2.5 O'
_chemical_formula_weight         487.13
_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                 99.838(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.5098(9)
_cell_length_b                   17.722(2)
_cell_length_c                   22.2233(9)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      11.05
_cell_volume                     6018.6(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      183(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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       17
_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            9304
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.21
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.7790
_exptl_absorpt_correction_T_min  0.3682
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.133
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_obs          0.0652
_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^)+(0.0575P)^2^+0.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1637
_refine_ls_wR_factor_obs         0.1320
_reflns_number_observed          5292
_reflns_number_total             8930
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om700611q-file002.cif
_cod_data_source_block           Compound_1a
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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^)+(0.0575P)^2^+0.5267P] 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^)+(0.0575P)^2^+0.5267P] 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        6018.7(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C28 H45.50 N2.50 O Al2'
_cod_database_code               4073771