Methylaluminoxane-Free Chromium Catalytic System for Ethylene Tetramerization.
Kim, Eun Ho; Lee, Hyun Mo; Jeong, Myoung Sun; Ryu, Ji Yeon; Lee, Junseong; Lee, Bun Yeoul; ACS omega 2 (2017) 765–773; doi:10.1021/acsomega.6b00506

data_4516837
_publ_section_title
;
 Methylaluminoxane-Free Chromium Catalytic System for Ethylene
 Tetramerization.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              765
_journal_page_last               773
_journal_paper_doi               10.1021/acsomega.6b00506
_journal_volume                  2
_journal_year                    2017
_chemical_formula_sum            'C40 H32 B Cl2 Cr F20 O4'
_chemical_formula_weight         1090.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0405(3)
_cell_length_b                   17.0405(3)
_cell_length_c                   28.3198(10)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.88
_cell_volume                     8223.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            25647
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.102
_diffrn_reflns_theta_min         1.438
_exptl_absorpt_coefficient_mu    0.543
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       block
_exptl_crystal_F_000             4376
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                3373
_reflns_number_total             4962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao6b00506_si_006.cif
_cod_data_source_block           lby88-5
_cod_database_code               4516837
_shelxl_version_number           2014-3
_shelx_res_checksum              68234
_shelx_hkl_checksum              24761