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_7042887
_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         'C31 H35 Cl3 Cr N3'
_chemical_formula_sum            'C31 H35 Cl3 Cr N3'
_chemical_formula_weight         607.97
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-18
_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                90.00
_cell_angle_beta                 105.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.671(3)
_cell_length_b                   13.380(3)
_cell_length_c                   16.481(3)
_cell_measurement_reflns_used    8593
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4754
_cell_measurement_theta_min      1.5442
_cell_volume                     2908.1(11)
_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
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.9000
_diffrn_measured_fraction_theta_max 27.4754
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.8707
              2theta: -19.9301
scan:
    Number of images: 346
               Slice: -110.0000 - 63.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.8707
              2theta: -19.9301
scan:
    Number of images: 278
               Slice: -76.2500 - 62.7500
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 44.8707
              2theta: -19.9301
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0569
_diffrn_orient_matrix_UB_12      -0.0296
_diffrn_orient_matrix_UB_13      0.0404
_diffrn_orient_matrix_UB_21      -0.0087
_diffrn_orient_matrix_UB_22      -0.0652
_diffrn_orient_matrix_UB_23      -0.0356
_diffrn_orient_matrix_UB_31      0.0519
_diffrn_orient_matrix_UB_32      0.0115
_diffrn_orient_matrix_UB_33      -0.0336
_diffrn_radiation_detector       CCD
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0302
_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       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30864
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87335
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.218
_platon_squeeze_details
;
;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+2.8755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                6315
_reflns_number_total             6649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01077j1.cif
_cod_data_source_block           Cr1
_cod_original_cell_volume        2908.0(10)
_cod_database_code               7042887
_diffrn_number_total             6965
_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:
 C13(H13A,H13B), C3(H3A,H3B), C10(H10A,H10B), C6(H6A,H6B), C4(H4A,H4B),
 C12(H12A,H12B), C5(H5A,H5B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C25(H25), C26(H26), C24(H24), C20(H20), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C27A(H27A,H27B,H27C), C17A(H17A,H17B,H17C), C23A(H23A,
 H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'