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_7044536
_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         'C57 H48 Br2 N2 Ni, C4 H10 O'
_chemical_formula_sum            'C61 H58 Br2 N2 Ni O'
_chemical_formula_weight         1053.62
_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
_atom_sites_solution_primary     dual
_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                 95.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.612(2)
_cell_length_b                   18.490(4)
_cell_length_c                   25.591(5)
_cell_measurement_reflns_used    14649
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4826
_cell_measurement_theta_min      1.3605
_cell_volume                     5002.3(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68422
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.598
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.84322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.986
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11424
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+5.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10748
_reflns_number_total             11424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03362a2.cif
_cod_data_source_block           1573416
_cod_original_cell_volume        5002.4(17)
_cod_database_code               7044536
_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. Restrained distances
 C3AA-C2AA
 2.5 with sigma of 0.04
3.a Ternary CH refined with riding coordinates:
 C20(H20), C32(H32), C45(H45)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C2AA(H2AA,
 H2AB), C3AA(H3AA,H3AB)
3.c Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00Z(H00Z), C1(H1), C01H(H01H), C01L(H01L), C01P(H01P), C2(H2),
 C3(H3), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C27(H27),
 C29(H29), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,
 H1AB,H1AC)
;
_shelx_res_checksum              30606
_olex2_submission_special_instructions 'No special instructions were received'