Preparation and Characterization of a Reduced Chromium Complex via Vinyl Oxidative Coupling: Formation of a Self-Activating Catalyst for Selective Ethylene Trimerization
Khalid Albahily; Valeria Fomitcheva; Sandro Gambarotta; Ilia Korobkov; Muralee Murugesu; Serge I. Gorelsky; Journal of the American Chemical Society 133 (2011) 6380–6387; doi:10.1021/ja200593k

data_4106041
_publ_section_title
;
 Preparation and Characterization of a Reduced Chromium Complex via Vinyl
 Oxidative Coupling: Formation of a Self-Activating Catalyst for Selective
 Ethylene Trimerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6380
_journal_page_last               6387
_journal_paper_doi               10.1021/ja200593k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C66.92 H91.33 Cr3 N6 P3'
_chemical_formula_weight         1228.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 99.206(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.868(3)
_cell_length_b                   27.799(6)
_cell_length_c                   17.357(4)
_cell_measurement_reflns_used    1631
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      5.62
_cell_volume                     7082(3)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         5.55
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             2607
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                4736
_reflns_number_total             7685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200593k_si_001.cif
_cod_data_source_block           sg3968sqz
_cod_database_code               4106041