An aza-cyclophane supported macrocyclic α-diimine nickel catalyst for ethylene polymerization
Yang, Jingshuang; Chi, Yue; Zhang, Yuxing; Jian, Zhongbao; Polymer Chemistry 15 (2024) 1530–1535; doi:10.1039/D3PY01402A

data_1571260
_publ_section_title
;
 An aza-cyclophane supported macrocyclic \a-diimine nickel catalyst for
 ethylene polymerization
;
_journal_issue                   15
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1530
_journal_page_last               1535
_journal_paper_doi               10.1039/D3PY01402A
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C50 H36 Br2 N6 Ni'
_chemical_formula_sum            'C50 H36 Br2 N6 Ni'
_chemical_formula_weight         935.34
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2h6kv4
_audit_creation_date             2022-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-10-10 deposited with the CCDC.	2024-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8543(4)
_cell_length_b                   22.0339(8)
_cell_length_c                   17.7751(7)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.221
_cell_measurement_theta_min      2.190
_cell_volume                     4530.3(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1138
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            118654
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.075
_diffrn_reflns_theta_min         1.988
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       needle
_exptl_crystal_F_000             1888
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         13263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0538P)^2^+4.7060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7810
_reflns_number_total             13263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01402a2.cif
_cod_data_source_block           mo_20221213_0m_sq
_cod_depositor_comments          'Adding full bibliography for 1571260.cif.'
_cod_database_code               1571260
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C21(H21), N3(H3), C50(H50), C37(H37), N5(H5), C46(H46), C4(H4A),
 C48(H48), C34(H34), C23(H23), C15(H15), C47(H47), C40(H40), C18(H18), C31(H31),
  C5(H5A), C10(H10), C24(H24), C25(H25), N6(H6), C6(H6A), C44(H44), C11(H11),
 C42(H42), C27(H27), C29(H29), C12(H12), C43(H43), C28(H28)
2.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              67140
_shelx_hkl_checksum              57787
_shelx_fab_checksum              80651
_olex2_submission_special_instructions 'No special instructions were received'