Highly branched unsaturated polyethylenes achievable using strained imino-cyclopenta[b]pyridyl-nickel precatalysts
Zhang, Youfu; Huang, Chuanbing; Wang, Xinxin; Mahmood, Qaiser; Hao, Xiang; Hu, Xinquan; Guo, Cun-Yue; Solan, Gregory A.; Sun, Wen-Hua; Polymer Chemistry 8 (2017) 995–; doi:10.1039/C6PY02089E

data_1553408
_publ_section_title
;
 Highly branched unsaturated polyethylenes achievable using strained
 imino-cyclopenta[b]pyridyl-nickel precatalysts
;
_journal_issue                   6
_journal_name_full               'Polymer Chemistry'
_journal_page_first              995
_journal_paper_doi               10.1039/C6PY02089E
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C36 H40 Cl2 N4 Ni'
_chemical_formula_sum            'C36 H40 Cl2 N4 Ni'
_chemical_formula_weight         658.31
_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_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0742(18)
_cell_length_b                   14.496(3)
_cell_length_c                   12.391(3)
_cell_measurement_reflns_used    4715
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4781
_cell_measurement_theta_min      1.4048
_cell_volume                     1613.9(6)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9906
_diffrn_measured_fraction_theta_max 0.9906
_diffrn_measurement_details
;
scan:
	Number of images: 300
	           Slice: -110.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0140
	          2theta: -19.9120
scan:
	Number of images: 300
	           Slice: -110.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0140
	          2theta: -19.9120
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0810
_diffrn_orient_matrix_UB_12      0.0228
_diffrn_orient_matrix_UB_13      -0.0729
_diffrn_orient_matrix_UB_21      0.0307
_diffrn_orient_matrix_UB_22      0.0403
_diffrn_orient_matrix_UB_23      0.0468
_diffrn_orient_matrix_UB_31      0.0504
_diffrn_orient_matrix_UB_32      -0.0610
_diffrn_orient_matrix_UB_33      0.0195
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10742
_diffrn_reflns_theta_full        27.4974
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8138
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             693.4891
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.4292
_refine_diff_density_min         -0.2673
_refine_diff_density_rms         0.0666
_refine_ls_d_res_high            0.7697
_refine_ls_d_res_low             6.8592
_refine_ls_goodness_of_fit_ref   1.0388
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    31
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0388
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.9852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -8
_reflns_number_gt                3542
_reflns_number_total             3674
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6py02089e2.cif
_cod_data_source_block           Ni1
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1553408
_diffrn_number_total             3844
_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 Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C1(H1), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C17(H17a,H17b,H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'