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_1546243
_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         'C60 H56 Cl N4 Ni, Al Cl4, 3/2(C H2 Cl2)'
_chemical_formula_sum            'C61.5 H59 Al Cl8 N4 Ni'
_chemical_formula_weight         1223.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                90
_cell_angle_beta                 101.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.975(8)
_cell_length_b                   15.547(6)
_cell_length_c                   24.680(12)
_cell_measurement_reflns_used    2987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.36
_cell_measurement_theta_min      2.62
_cell_volume                     6373(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2011
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_unetI/netI     0.2091
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51534
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.049
_diffrn_reflns_theta_min         0.843
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3126 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         23143
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2091
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                11349
_reflns_number_total             23143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy00875a2.cif
_cod_data_source_block           6
_cod_depositor_comments
;

2019-03-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C123 H118 Al2 Cl16 N8 Ni2'
_cod_original_formula_weight         2446.83
_cod_original_formula_moiety      '2(C60 H56 Cl N4 Ni), 2(Al Cl4), 3(C H2 Cl2)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1546243
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              22281