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_7044535
_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'
_chemical_formula_sum            'C58 H50 Br2 N2 Ni'
_chemical_formula_weight         993.53
_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             2017-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.658(2)
_cell_length_b                   18.896(4)
_cell_length_c                   25.117(5)
_cell_measurement_reflns_used    14484
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4807
_cell_measurement_theta_min      1.3506
_cell_volume                     5037.7(18)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         1.351
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.63873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         11483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0387P)^2^+5.0387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10622
_reflns_number_total             11483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03362a2.cif
_cod_data_source_block           Ni1
_cod_original_cell_volume        5037.8(18)
_cod_database_code               7044535
_shelx_shelxl_version_number     2017/1
_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:
 C32(H32), C45(H45), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C21(H21A,H21B), C23(H23A,H23B), C20(H20A,H20B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C8(H8), C30(H30), C10(H10), C3AA(H3AA), C28(H28), C40(H40),
 C9(H9), C5(H5), C57(H57), C15(H15), C47(H47), C16(H16), C48(H48), C17(H17),
 C34(H34), C44(H44), C54(H54), C51(H51), C41(H41), C42(H42), C53(H53), C49(H49),
  C55(H55), C38(H38), C50(H50), C37(H37), C56(H56), C43(H43), C36(H36), C35(H35)
2.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              79234
_shelx_fab_checksum              17725
_olex2_submission_special_instructions 'No special instructions were received'