From Polyethylene Waxes to HDPE using a α,α'-Bis(arylimino)- 2,3:5,6-bis(pentamethylene)pyridyl-Chromium(III) Chloride Pre-catalyst in Ethylene Polymerisation
Huang, Chuanbing; Du, Shizhen; Solan, Gregory; Sun, Yang; Sun, Wen Hua; Dalton Trans.  (2017) –; doi:10.1039/C7DT01077J

data_7042886
_publ_section_title
;
 From Polyethylene Waxes to HDPE using a \a,\a'-Bis(arylimino)-
 2,3:5,6-bis(pentamethylene)pyridyl-Chromium(III) Chloride Pre-catalyst in
 Ethylene Polymerisation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01077J
_journal_year                    2017
_chemical_formula_moiety         'C33 H39 Cl3 Cr N3, 2(C H2 Cl2)'
_chemical_formula_sum            'C35 H43 Cl7 Cr N3'
_chemical_formula_weight         805.92
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-03-19 deposited with the CCDC.
2017-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.544(3)
_cell_length_b                   12.665(3)
_cell_length_c                   18.291(4)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4790
_cell_measurement_theta_min      1.1185
_cell_volume                     3814.8(14)
_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 99.7000
_diffrn_measured_fraction_theta_max 27.4790
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 44.9393
              2theta: -19.8911
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9393
              2theta: -19.8911
scan:
    Number of images: 286
               Slice: -110.0000 - 33.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9393
              2theta: -19.8911
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0041
_diffrn_orient_matrix_UB_12      0.0205
_diffrn_orient_matrix_UB_13      -0.0570
_diffrn_orient_matrix_UB_21      0.0787
_diffrn_orient_matrix_UB_22      -0.0048
_diffrn_orient_matrix_UB_23      0.0039
_diffrn_orient_matrix_UB_31      -0.0019
_diffrn_orient_matrix_UB_32      -0.0496
_diffrn_orient_matrix_UB_33      -0.0236
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41032
_diffrn_reflns_theta_full        27.4678
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.4031
_exptl_crystal_description       plate
_exptl_crystal_F_000             1673.8534
_exptl_crystal_size_max          0.807
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.9982
_refine_diff_density_min         -1.3476
_refine_diff_density_rms         0.1621
_refine_ls_d_res_high            0.7704
_refine_ls_d_res_low             10.3969
_refine_ls_goodness_of_fit_ref   1.0355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0355
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+10.2431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8423
_reflns_number_total             8697
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt01077j1.cif
_cod_data_source_block           Cr4
_cod_original_cell_volume        3814.9(13)
_cod_database_code               7042886
_diffrn_number_total             9101
_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:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C13(H13a,H13b), C6(H6a,H6b), C10(H10a,
 H10b), C11(H11a,H11b), C12(H12a,H12b), C61(H61a,H61b), C0AA(H0Aa,H0Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C8(H8), C26(H26), C24(H24)
2.c Idealised Me refined as rotating group:
 C21a(H21a,H21b,H21c), C17a(H17a,H17b,H17c), C19a(H19a,H19b,H19c), C23a(H23a,
 H23b,H23c), C25a(H25a,H25b,H25c), C27a(H27a,H27b,H27c)
;
_olex2_submission_special_instructions 'No special instructions were received'