Synthesis of bis-(benzocyclohexan-ketoimino) Ni(ii) with different electron groups and their catalytic copolymerization of norbornene and polar norbornene
He, Xiaohui; Yang, Yingping; Wang, Suli; Han, Zhilong; Tu, Guangshui; Zhang, Feng; Huang, Shengmei; Wang, Zijie; Chen, Defu; RSC Adv. 7 (2017) 48745–; doi:10.1039/C7RA09944D

data_7229355
_publ_section_title
;
 Synthesis of bis-(benzocyclohexan-ketoimino) Ni(ii) with different
 electron groups and their catalytic copolymerization of norbornene and
 polar norbornene
;
_journal_issue                   77
_journal_name_full               'RSC Adv.'
_journal_page_first              48745
_journal_paper_doi               10.1039/C7RA09944D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C38 H36 N2 Ni O4'
_chemical_formula_sum            'C38 H36 N2 Ni O4'
_chemical_formula_weight         643.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.988(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6652(13)
_cell_length_b                   14.8520(13)
_cell_length_c                   7.0027(6)
_cell_measurement_reflns_used    7299
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.002
_cell_measurement_theta_min      3.108
_cell_volume                     1519.5(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9759
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.108
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1056 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.7447.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0369P)^2^+0.4989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2352
_reflns_number_total             2810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09944d1.cif
_cod_data_source_block           20160108d_0m_pl
_cod_database_code               7229355
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'