Lewis acids in situ modulate pyridazine-imine Ni catalysed ethylene (co)polymerisation
Wang, Guohong; Li, Min; Pang, Wenmin; Chen, Min; Tan, Chen; New Journal of Chemistry 43 (2019) 13630–; doi:10.1039/C9NJ01243E

data_7058761
_publ_section_title
;
 Lewis acids in situ modulate pyridazine-imine Ni catalysed ethylene
 (co)polymerisation
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13630
_journal_paper_doi               10.1039/C9NJ01243E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C22 H30 Br2 Cl N3 Ni O, 1[H2O]'
_chemical_formula_sum            'C22 H32 Br2 Cl N3 Ni O2'
_chemical_formula_weight         624.48
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5796)
;
_audit_update_record
;
2019-07-24 deposited with the CCDC.    2019-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.206(5)
_cell_length_b                   23.206(5)
_cell_length_c                   8.801(5)
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    273
_cell_measurement_theta_max      22.03
_cell_measurement_theta_min      2.31
_cell_volume                     4105(3)
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.755
_exptl_absorpt_coefficient_mu    3.749
_exptl_absorpt_correction_T_max  0.475
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker;SADABS;2012
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2675
_reflns_number_total             4837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01243e2.cif
_cod_data_source_block           ni1
_cod_depositor_comments          'Adding full bibliography for 7058761.cif.'
_cod_database_code               7058761
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.399
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O1, C19B, C22B, C21A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C20B, C22A, C21B, C19A, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(C20B)=
 Sof(H20A)=Sof(H20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=1-FVAR(1)
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C20A)=
 Sof(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C19B(H19A,H19B), C22B(H22A,H22B), C20B(H20A,H20B), C21B(H21A,H21B), C22A(H22C,
 H22D), C21A(H21C,H21D), C20A(H20C,H20D), C19A(H19C,H19D)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C3(H3), C9(H9), C10(H10)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C17(H17A,H17B,H17C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 59 electrons were
found in a volume of 356\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 1[H2O] per
Formula Unit which account for 60 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5892
_shelx_fab_checksum              27734
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'