Nickel-catalyzed direct synthesis of hyperbranched liquid oligoethylene
Zhang, Mengyao; Dai, Shengyu; Polymer Chemistry 15 (2024) 4627–4636; doi:10.1039/D4PY00709C

data_1572857
_publ_section_title
;
 Nickel-catalyzed direct synthesis of hyperbranched liquid oligoethylene
;
_journal_issue                   45
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4627
_journal_page_last               4636
_journal_paper_doi               10.1039/D4PY00709C
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C31 H41 Br3 N2 Ni, 0.1[H2O]'
_chemical_formula_sum            'C31 H41 Br3 N2 Ni O2'
_chemical_formula_weight         772.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-07-19 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.8140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9221(2)
_cell_length_b                   18.1077(2)
_cell_length_c                   21.0075(3)
_cell_measurement_reflns_used    20487
_cell_measurement_temperature    296.93(10)
_cell_measurement_theta_max      77.4410
_cell_measurement_theta_min      2.1880
_cell_volume                     6925.49(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.93(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_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    -61.00 -33.00   0.50    0.80    -- -104.50  57.00  60.00   56
  2  \w    -62.00 -33.00   0.50    0.80    -- -104.50  57.00-120.00   58
  3  \w    -62.00 -33.00   0.50    0.80    -- -104.50  57.00-150.00   58
  4  \w    -58.00 -32.00   0.50    0.80    -- -104.50  57.00-180.00   52
  5  \w    -19.00  24.00   0.50    0.20    --  -49.58  19.00-150.00   86
  6  \w    -22.00  11.00   0.50    0.20    --  -49.58  19.00-180.00   66
  7  \w    -22.00  13.00   0.50    0.20    --  -49.58  19.00 -60.00   70
  8  \w     26.00  51.00   0.50    0.20    --   49.58-116.00 -74.00   50
  9  \w     58.00  83.00   0.50    0.20    --   49.58-167.00 139.00   50
 10  \w     67.00  92.00   0.50    0.80    --  106.85-167.00 139.00   50
 11  \w     66.00  92.00   0.50    0.80    --  106.85-116.00 -74.00   52
 12  \w     40.00 102.00   0.50    0.80    --  106.85 -99.00 -90.00  124
 13  \w     36.00 108.00   0.50    0.80    --  106.85 -77.00 -90.00  144
 14  \w     39.00  68.00   0.50    0.80    --  106.85 -57.00 -90.00   58
 15  \w     37.00  69.00   0.50    0.80    --  106.85 -57.00 -60.00   64
 16  \w     37.00  66.00   0.50    0.80    --  106.85 -57.00 -30.00   58
 17  \w     35.00  66.00   0.50    0.80    --  106.85 -57.00 120.00   62
 18  \w    -20.00  44.00   0.50    0.20    --   49.58 -38.00 150.00  128
 19  \w    102.00 152.00   0.50    0.80    --  106.85  19.00 120.00  100
 20  \w   -111.00 -78.00   0.50    0.20    --  -49.58 167.00 159.00   66
 21  \w   -102.00 -77.00   0.50    0.80    -- -104.50 116.00  13.00   50
 22  \w   -111.00 -39.00   0.50    0.80    -- -104.50 125.00 -30.00  144
 23  \w     60.00 122.00   0.50    0.20    --   49.58 167.00 159.00  124
 24  \w    106.00 131.00   0.50    0.80    --  106.85 116.00  13.00   50
 25  \w   -174.00 -98.00   0.50    0.80    -- -104.50 -38.00 120.00  152
 26  \w   -106.00 -81.00   0.50    0.80    -- -104.50-167.00 139.00   50
 27  \w   -114.00 -49.00   0.50    0.20    --  -49.58-167.00 139.00  130
 28  \w   -171.00 -80.00   0.50    0.80    -- -104.50-116.00 -74.00  182
;
_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      -0.0163583000
_diffrn_orient_matrix_UB_12      0.0726731000
_diffrn_orient_matrix_UB_13      -0.0393702000
_diffrn_orient_matrix_UB_21      -0.0019330000
_diffrn_orient_matrix_UB_22      -0.0421136000
_diffrn_orient_matrix_UB_23      -0.0641755000
_diffrn_orient_matrix_UB_31      -0.0830150000
_diffrn_orient_matrix_UB_32      -0.0133790000
_diffrn_orient_matrix_UB_33      -0.0119232000
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27208
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.102
_diffrn_reflns_theta_min         3.707
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear bluish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.446
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0486
_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^)+(0.1038P)^2^+11.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6573
_reflns_number_total             7105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00709c2.cif
_cod_data_source_block           zmy_auto
_cod_depositor_comments          'Adding full bibliography for 1572857.cif.'
_cod_database_code               1572857
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Br Ni'
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C21(H21), C10(H10), C27(H27)
1.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C15(H15A,H15B), C25(H25A,H25B), C11(H11A,
 H11B), C28(H28A,H28B), C32(H32A,H32B), C30(H30A,H30B), C14(H14A,H14B),
 C31(H31A,H31B), C23(H23A,H23B), C12(H12A,H12B), C24(H24A,H24B), C29(H29A,H29B),
  C13(H13A,H13B)
1.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C4(H4), C2(H2), C3(H3)
1.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_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 2.498
_oxdiff_exptl_absorpt_empirical_full_min 0.412