Reactivity of cationic α-diimine cyclopentadienyl nickel complexes towards AlEt2Cl: Synthesis, characterisation and ethylene polymerisation
Gomes, Pedro T.; Gomes, Clara S. B.; Ribeiro, Alejandro F. G.; Fernandes, Anabela C.; Bento, Artur; do Rosário Ribeiro, Maria; Pascu, Sofia I.; Kociok-Kohn, Gabriele; Duarte, Maria Teresa Teresa; Catal. Sci. Technol.  (2017) –; doi:10.1039/C7CY00875A

data_1546244
_publ_section_title
;
 Reactivity of cationic \a-diimine cyclopentadienyl nickel complexes
 towards AlEt2Cl: Synthesis, characterisation and ethylene polymerisation
;
_journal_name_full               'Catal. Sci. Technol.'
_journal_paper_doi               10.1039/C7CY00875A
_journal_year                    2017
_chemical_formula_moiety         'C90 H84 Cl5 N6 Ni3, Al Cl4'
_chemical_formula_sum            'C90 H84 Al Cl9 N6 Ni3'
_chemical_formula_weight         1771.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                112.115(9)
_cell_angle_beta                 101.465(10)
_cell_angle_gamma                100.432(11)
_cell_formula_units_Z            2
_cell_length_a                   14.507(3)
_cell_length_b                   16.966(3)
_cell_length_c                   19.647(4)
_cell_measurement_reflns_used    68728
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.17
_cell_volume                     4212.5(15)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.1249
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68728
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.204
_diffrn_reflns_theta_max         25.204
_diffrn_reflns_theta_min         1.170
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         14755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.2102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8407
_reflns_number_total             14755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy00875a2.cif
_cod_data_source_block           5
_cod_original_cell_volume        4212.4(14)
_cod_database_code               1546244
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              72910