ortho-Cycloalkyl substituted N,N′-diaryliminoacenaphthene-Ni(ii) catalysts for polyethylene elastomers; exploring ring size and temperature effects
Suo, Hongyi; Oleynik, Irina V.; Huang, Chuanbing; Oleynik, Ivan I.; Solan, Gregory A.; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Dalton Trans.  (2017) –; doi:10.1039/C7DT03362A

data_7044537
_publ_section_title
;
 ortho-Cycloalkyl substituted N,N&#x2032;-diaryliminoacenaphthene-Ni(ii)
 catalysts for polyethylene elastomers; exploring ring size and
 temperature effects
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03362A
_journal_year                    2017
_chemical_formula_moiety         'C58 H50 Br2 N2 Ni, C4 H10 O'
_chemical_formula_sum            'C62 H60 Br2 N2 Ni O'
_chemical_formula_weight         1067.61
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.526(2)
_cell_length_b                   17.767(4)
_cell_length_c                   27.812(6)
_cell_measurement_reflns_used    13926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4811
_cell_measurement_theta_min      1.3614
_cell_volume                     5183.6(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            70411
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208.0
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         11865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+7.2649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                11332
_reflns_number_total             11865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03362a2.cif
_cod_data_source_block           Ni5
_cod_original_cell_volume        5183.5(18)
_cod_database_code               7044537
_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 Ternary CH refined with riding coordinates:
 C19(H19), C46(H46), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C61(H61A,
 H61B), C60(H60A,H60B)
2.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C28(H28), C58(H58), C35(H35), C37(H37), C10(H10), C40(H40),
 C17(H17), C30(H30), C3(H3), C4(H4), C15(H15), C36(H36), C52(H52), C38(H38),
 C44(H44), C42(H42), C41(H41), C48(H48), C5(H5), C54(H54), C56(H56), C8(H8),
 C9(H9), C55(H55), C50(H50), C57(H57), C43(H43), C49(H49), C51(H51)
2.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C59(H59A,H59B,
 H59C), C62(H62A,H62B,H62C)
;
_olex2_submission_special_instructions 'No special instructions were received'