Achieving polydispersive HDPE by N,N,N-Co precatalysts appended with N-2,4-bis(di(4-methoxyphenyl)methyl)-6-methylphenyl
Yuan, Shi-Fang; Fan, Zhe; Yan, Yi; Ma, Yanping; Han, Mingyang; Liang, Tongling; Sun, Wen-Hua; RSC Advances 10 (2020) 43400–43411; doi:10.1039/D0RA09333E

data_7241789
_publ_section_title
;
 Achieving polydispersive HDPE by N,N,N-Co precatalysts appended with
 N-2,4-bis(di(4-methoxyphenyl)methyl)-6-methylphenyl
;
_journal_issue                   71
_journal_name_full               'RSC Advances'
_journal_page_first              43400
_journal_page_last               43411
_journal_paper_doi               10.1039/D0RA09333E
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C55 H55 Cl2 Co N3 O4'
_chemical_formula_sum            'C55 H55 Cl2 Co N3 O4'
_chemical_formula_weight         951.91
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-09-04 deposited with the CCDC.	2020-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.564(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3277(3)
_cell_length_b                   15.5549(4)
_cell_length_c                   26.3520(7)
_cell_measurement_reflns_used    12571
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      73.2680
_cell_measurement_theta_min      3.2770
_cell_volume                     4996.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9605
_diffrn_measured_fraction_theta_max 0.9605
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -118.00 -85.00   0.50    0.44    --  -46.95-122.00  63.00   66
  2  \w    -70.00 -37.00   0.50    0.44    --  -46.95 122.00 144.00   66
  3  \w    -86.00 -61.00   0.50    0.44    --  -46.95-151.00 -98.00   50
  4  \w     17.00  92.00   0.50    0.44    --   46.95-122.00  63.00  150
  5  \w     46.00  71.00   0.50    0.44    --   46.95-151.00 -98.00   50
  6  \w   -145.00-120.00   0.50    1.50    --  -99.00-122.00  63.00   50
  7  \w   -105.00 -80.00   0.50    1.50    --  -99.00 151.00 -54.00   50
  8  \w     31.00 131.00   0.50    1.50    --  103.25-151.00 -98.00  200
  9  \w    100.00 168.00   0.50    1.50    --  103.25 122.00 144.00  136
 10  \w     72.00 107.00   0.50    1.50    --  103.25-122.00  63.00   70
 11  \w   -118.00 -80.00   0.50    0.44    --  -46.95-125.00 120.00   76
 12  \w   -119.00 -56.00   0.50    0.44    --  -46.95 -77.00  90.00  126
 13  \w     35.00 115.00   0.50    0.44    --   46.95  38.00-120.00  160
 14  \w   -168.00-109.00   0.50    1.50    --  -99.00 -30.00  60.00  118
 15  \w    -93.00 -32.00   0.50    1.50    --  -99.00  45.00   0.00  122
 16  \w     35.00  70.00   0.50    1.50    --  103.25 -94.00 150.00   70
 17  \w     31.00 109.00   0.50    1.50    --  103.25 -94.00  60.00  156
 18  \w     35.00 108.00   0.50    1.50    --  103.25 -94.00 -90.00  146
 19  \w    100.00 168.00   0.50    1.50    --  103.25  45.00  90.00  136
 20  \w     32.00 103.00   0.50    1.50    --  103.25 -94.00-120.00  142
 21  \w     92.00 156.00   0.50    1.50    --  103.25  45.00-120.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0877898000
_diffrn_orient_matrix_UB_12      -0.0232591000
_diffrn_orient_matrix_UB_13      0.0336505000
_diffrn_orient_matrix_UB_21      -0.0304558000
_diffrn_orient_matrix_UB_22      0.0957042000
_diffrn_orient_matrix_UB_23      0.0029871000
_diffrn_orient_matrix_UB_31      -0.0856833000
_diffrn_orient_matrix_UB_32      -0.0102512000
_diffrn_orient_matrix_UB_33      -0.0485172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38554
_diffrn_reflns_theta_full        75.7663
_diffrn_reflns_theta_max         75.77
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.2652
_exptl_crystal_description       needle
_exptl_crystal_F_000             1994.5887
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.1040
_refine_diff_density_min         -0.4580
_refine_diff_density_rms         0.0755
_refine_ls_d_res_high            0.7953
_refine_ls_d_res_low             13.3563
_refine_ls_goodness_of_fit_ref   1.2723
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     596
_refine_ls_number_reflns         9991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.2723
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                7938
_reflns_number_total             9991
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra09333e2.cif
_cod_data_source_block           Co4
_cod_database_code               7241789
_chemical_oxdiff_usercomment     'C H N Coi Cl O'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C41(H41), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C24(H24), C22(H22), C28(H28), C29(H29), C31(H31),
 C32(H32), C35(H35), C36(H36), C38(H38), C39(H39), C47(H47), C46(H46), C44(H44),
  C43(H43), C54(H54), C53(H53), C51(H51), C50(H50), C6(H6), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C18(H18a,H18b,H18c), C17(H17a,H17b,
 H17c), C9(H9a,H9b,H9c), C16(H16a,H16b,H16c), C48(H48a,H48b,H48c), C33(H33a,
 H33b,H33c), C40(H40a,H40b,H40c), C55(H55a,H55b,H55c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.422