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_7229354
_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 H30 F6 N2 Ni O2'
_chemical_formula_sum            'C38 H30 F6 N2 Ni O2'
_chemical_formula_weight         719.35
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.484(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.719(3)
_cell_length_b                   7.351(3)
_cell_length_c                   24.392(10)
_cell_measurement_reflns_used    3482
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.610
_cell_measurement_theta_min      3.239
_cell_volume                     1558.6(10)
_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      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8579
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.795
_diffrn_reflns_theta_max         24.795
_diffrn_reflns_theta_min         3.239
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1105 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8463.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0055(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2618
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0958
_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^)+(0.0227P)^2^+21.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1984
_reflns_number_total             2618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09944d1.cif
_cod_data_source_block           20160111a_0m_pl
_cod_database_code               7229354
_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. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'