Bis(N-acylated imidazolin-2-imine) nickel catalyzed norbornene copolymerization with methyl acrylate
Li, Yanqing; Zhang, Hu; Xiao, Ru; Cai, Zhengguo; Polymer Chemistry 11 (2020) 5542–5547; doi:10.1039/D0PY00857E

data_1558685
_publ_section_title
;
 Bis(N-acylated imidazolin-2-imine) nickel catalyzed norbornene
 copolymerization with methyl acrylate
;
_journal_issue                   34
_journal_name_full               'Polymer Chemistry'
_journal_page_first              5542
_journal_page_last               5547
_journal_paper_doi               10.1039/D0PY00857E
_journal_volume                  11
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C44 H32 N6 Ni O2'
_chemical_formula_sum            'C44 H32 N6 Ni O2'
_chemical_formula_weight         735.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-05 deposited with the CCDC.	2020-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.982(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8938(18)
_cell_length_b                   19.286(3)
_cell_length_c                   10.6047(19)
_cell_measurement_reflns_used    2342
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      52.995
_cell_measurement_theta_min      4.071
_cell_volume                     1803.2(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      169.98
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.1612
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9115
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.468
_diffrn_reflns_theta_min         4.070
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.243
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1341 before and 0.0967 after correction. The Ratio of minimum to maximum transmission is 0.6383. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.072(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                3062
_reflns_number_total             5790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py00857e2.cif
_cod_data_source_block           wmj18123_0m
_cod_depositor_comments
;
 Adding full bibliography for 1558683--1558686.cif.

2022-06-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.5(C44 H32 N6 Ni O2)'
_cod_original_formula_sum        'C22 H16 N3 Ni0.50 O'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     367.73
_cod_database_code               1558685
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.928(13)
 0.072(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
;
_shelx_res_checksum              40441
_olex2_submission_special_instructions 'No special instructions were received'