Synthesis of hyperbranched low molecular weight polyethylene oils by an iminopyridine nickel(II) catalyst
D'Auria, Ilaria; Milione, Stefano; Caruso, Tonino; Balducci, Gabriele; Pellecchia, Claudio; Polym. Chem.  (2017) –; doi:10.1039/C7PY01215B

data_1547540
_publ_section_title
;
 Synthesis of hyperbranched low molecular weight polyethylene oils by an
 iminopyridine nickel(II) catalyst
;
_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY01215B
_journal_year                    2017
_chemical_formula_moiety         'C26 H30 Br2 N2 Ni, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C26.5 H31 Br2 Cl N2 Ni'
_chemical_formula_weight         631.51
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2017-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.079(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.210(6)
_cell_length_b                   14.5610(10)
_cell_length_c                   14.9960(17)
_cell_measurement_reflns_used    14914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.941
_cell_measurement_theta_min      1.503
_cell_volume                     2914.3(13)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  'private software'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
;
Huber 4-circles Kappa Goniometer, Pilatus 2M detector
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0091
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65998
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.941
_diffrn_reflns_theta_min         1.503
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    3.382
_exptl_absorpt_correction_T_max  1.449
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       prism
_exptl_crystal_F_000             1276
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, n-hexane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0069(6)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5145
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0721P)^2^+5.2465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4696
_reflns_number_total             5145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py01215b2.cif
_cod_data_source_block           lunn1-nibr2-06
_cod_original_cell_volume        2914.3(12)
_cod_original_formula_sum        'C26.50 H31 Br2 Cl N2 Ni'
_cod_database_code               1547540
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.728
_shelx_res_checksum              23076