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_7044538
_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         'C60 H54 Br2 N2 Ni, C H2 Cl2'
_chemical_formula_sum            'C61 H56 Br2 Cl2 N2 Ni'
_chemical_formula_weight         1106.51
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                102.42(3)
_cell_angle_beta                 93.70(3)
_cell_angle_gamma                93.95(3)
_cell_formula_units_Z            2
_cell_length_a                   10.987(2)
_cell_length_b                   12.500(3)
_cell_length_c                   19.151(4)
_cell_measurement_reflns_used    8957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.5897
_cell_measurement_theta_min      1.6743
_cell_volume                     2554.0(10)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28595
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.09
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         11649
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+2.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                10619
_reflns_number_total             11649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03362a2.cif
_cod_data_source_block           Ni3
_cod_original_cell_volume        2553.9(9)
_cod_database_code               7044538
_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. Restrained distances
 Cl1-C60 = Cl2-C61 = Cl3-C60 = Cl4-C61
 1.77 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl3 \\sim C60 \\sim C61 \\sim Cl2 \\sim Cl4: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl1) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(Cl2)=Sof(Cl4)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl3)=Sof(C60)=Sof(H60A)=Sof(H60B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA), C34(H34), C47(H47)
5.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C24(H24A,H24B), C23(H23A,H23B), C22(H22A,H22B), C21(H21A,
 H21B), C20(H20A,H20B), C19(H19A,H19B), C60(H60A,H60B), C61(H61A,H61B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C8(H8), C5(H5), C4(H4), C3(H3), C15(H15), C16(H16),
 C17(H17), C31(H31), C29(H29), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C40(H40), C39(H39), C38(H38), C37(H37), C36(H36), C55(H55), C56(H56),
 C57(H57), C58(H58), C59(H59), C53(H53), C52(H52), C51(H51), C50(H50), C49(H49)
5.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'