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_1546245
_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         'C27 H33 N2 Ni, 0.875(C6 H4 Cl2), C2 H5 Al Cl3'
_chemical_formula_sum            'C34.25 H41.5 Al Cl4.75 N2 Ni'
_chemical_formula_weight         735.27
_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_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-2016/6
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.8580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.65200(10)
_cell_length_b                   23.84300(10)
_cell_length_c                   12.7390(2)
_cell_measurement_reflns_used    3353
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.53
_cell_measurement_theta_min      2.26
_cell_volume                     3774.07(7)
_computing_cell_refinement       'Bruker SAINT (Bruker AXS, 1994)'
_computing_data_collection       'Bruker SMART (Bruker AXS, 1994)'
_computing_data_reduction        'Bruker SAINT (Bruker AXS, 1994)'
_computing_molecular_graphics    'ORTEP and Mercury'
_computing_publication_material  enCIFer
_computing_structure_refinement
;
 SHELXL-2016/6 (Sheldrick, 2016)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice \w-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6771
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22526
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        20.892
_diffrn_reflns_theta_max         20.892
_diffrn_reflns_theta_min         1.983
_diffrn_source                   'Daresbury SRS, Station 9.8'
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             1531
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         9232
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+2.9485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1841
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6987
_reflns_number_total             9232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy00875a2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C34.25 H41.50 Al Cl4.75 N2 Ni'
_cod_database_code               1546245
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              95853