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_7241788
_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         'C56 H57 Cl2 Co N3 O4'
_chemical_formula_sum            'C56 H57 Cl2 Co N3 O4'
_chemical_formula_weight         965.87
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-06
_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                 98.6430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2177(2)
_cell_length_b                   16.0747(2)
_cell_length_c                   25.6600(3)
_cell_measurement_reflns_used    14298
_cell_measurement_temperature    169.98(11)
_cell_measurement_theta_max      75.0910
_cell_measurement_theta_min      3.2430
_cell_volume                     4982.29(12)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.954
_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 -35.00   0.50    0.23    --  -47.20 -45.00 -85.00  166
  2  \w    -60.00  24.00   0.50    0.23    --  -47.20  45.00  64.00  168
  3  \w     57.00  83.00   0.50    0.23    --   47.20  45.00  64.00   52
  4  \w     -5.00  25.00   0.50    0.23    --   47.20 -45.00 -85.00   60
  5  \w    -71.00 -45.00   0.50    0.60    --  -99.00  45.00  64.00   52
  6  \w   -121.00 -90.00   0.50    0.60    --  -99.00 -45.00 -85.00   62
  7  \w    106.00 131.00   0.50    0.60    --  103.25  45.00  64.00   50
  8  \w     37.00 114.00   0.50    0.60    --  103.25 -45.00 -85.00  154
  9  \w     26.00  89.00   0.50    0.23    --   47.20-125.00-180.00  126
 10  \w   -103.00 -48.00   0.50    0.60    --  -99.00  15.00 -90.00  110
 11  \w   -115.00 -27.00   0.50    0.60    --  -99.00  61.00 -90.00  176
 12  \w   -107.00 -27.00   0.50    0.60    --  -99.00  45.00 -90.00  160
 13  \w   -109.00 -28.00   0.50    0.60    --  -99.00  30.00-120.00  162
 14  \w     52.00 125.00   0.50    0.60    --  103.25 -77.00-180.00  146
 15  \w     92.00 150.00   0.50    0.60    --  103.25  45.00  30.00  116
 16  \w     91.00 169.00   0.50    0.60    --  103.25  45.00 -60.00  156
 17  \w     92.00 168.00   0.50    0.60    --  103.25  30.00  60.00  152
;
_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      -0.0992228000
_diffrn_orient_matrix_UB_12      -0.0528059000
_diffrn_orient_matrix_UB_13      0.0111223000
_diffrn_orient_matrix_UB_21      0.0382668000
_diffrn_orient_matrix_UB_22      0.0094580000
_diffrn_orient_matrix_UB_23      0.0596879000
_diffrn_orient_matrix_UB_31      -0.0705543000
_diffrn_orient_matrix_UB_32      0.0793577000
_diffrn_orient_matrix_UB_33      0.0002682000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36867
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.590
_diffrn_reflns_theta_min         3.255
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43830
_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    1.288
_exptl_crystal_description       needle
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0690P)^2^+5.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8088
_reflns_number_total             9876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09333e2.cif
_cod_data_source_block           Co2
_cod_database_code               7241788
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Cl Co 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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C18(H18a,H18b)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C6(H6), C44(H44), C35(H35), C4(H4), C47(H47), C43(H43),
 C39(H39), C38(H38), C46(H46), C36(H36), C31(H31), C32(H32), C5(H5), C13(H13),
 C55(H55), C28(H28), C12(H12), C50(H50), C14(H14), C29(H29), C54(H54), C51(H51)
2.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C56(H56a,H56b,H56c), C9(H9a,H9b,H9c), C40(H40a,H40b,H40c),
 C48(H48a,H48b,H48c), C19(H19a,H19b,H19c), C33(H33a,H33b,H33c), C53(H53a,H53b,
 H53c), C17(H17a,H17b,H17c)
;
_shelx_res_checksum              72673
_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 1.931
_oxdiff_exptl_absorpt_empirical_full_min 0.520