Role of the metal oxidation state in the SNS-Cr catalyst for ethylene trimerization: isolation of di- and trivalent cationic intermediates.
Jabri, Amir; Temple, Claire; Crewdson, Patrick; Gambarotta, Sandro; Korobkov, Ilia; Duchateau, Robbert; Journal of the American Chemical Society 128 (2006) 9238–9247; doi:10.1021/ja0623717

data_4101324
_publ_section_title
;
 Role of the metal oxidation state in the SNS-Cr catalyst for ethylene
 trimerization: isolation of di- and trivalent cationic intermediates.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9238
_journal_page_last               9247
_journal_paper_doi               10.1021/ja0623717
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C26.5 H43 Al Cl6 Cr N S2'
_chemical_formula_weight         731.42
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.261(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8236(18)
_cell_length_b                   29.167(5)
_cell_length_c                   11.750(2)
_cell_measurement_reflns_used    207
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      19.78
_cell_measurement_theta_min      1.40
_cell_volume                     3595.1(10)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16310
_diffrn_reflns_theta_full        19.78
_diffrn_reflns_theta_max         19.78
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+9.4861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                2183
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0623717si20060406_014643.cif
_cod_data_source_block           sg2914
_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:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C26.50 H43 Al Cl6 Cr N S2'
_cod_database_code               4101324