Steric and electronic modulation of an iron catalyst as a route to remarkably high molecular weight linear polyethylene
Zhang, Randi; Han, Mingyang; Ma, Yanping; Solan, Gregory; tongling, liang; Sun, Wen Hua; Dalton Transactions  (2019) –; doi:10.1039/C9DT03880A

data_7701829
_publ_section_title
;
 Steric and electronic modulation of an iron catalyst as a route to
 remarkably high molecular weight linear polyethylene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03880A
_journal_year                    2019
_chemical_formula_moiety         'C49 H38 Cl2 F4 Fe N4 O2, 2.5[C4 H10 O]'
_chemical_formula_sum            'C59 H63 Cl2 F4 Fe N4 O4.5'
_chemical_formula_weight         1102.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-25 deposited with the CCDC.	2019-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                70.5393(15)
_cell_angle_beta                 77.3014(14)
_cell_angle_gamma                74.3520(15)
_cell_formula_units_Z            6
_cell_length_a                   19.2595(3)
_cell_length_b                   20.5620(4)
_cell_length_c                   24.3020(4)
_cell_measurement_reflns_used    28820
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.9920
_cell_measurement_theta_min      1.6950
_cell_volume                     8647.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)')'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_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_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -110.00  70.00   0.50   12.00    --  -20.00  45.00 270.00  360
  2  \w   -110.00  59.00   0.50   12.00    --  -20.00  45.00  90.00  338
  3  \w    -80.00  61.00   0.50   12.00    --  -20.00  45.00 180.00  282
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0246793000
_diffrn_orient_matrix_UB_12      0.0226608000
_diffrn_orient_matrix_UB_13      -0.0069935000
_diffrn_orient_matrix_UB_21      0.0290541000
_diffrn_orient_matrix_UB_22      -0.0298143000
_diffrn_orient_matrix_UB_23      0.0064829000
_diffrn_orient_matrix_UB_31      0.0063371000
_diffrn_orient_matrix_UB_32      -0.0003447000
_diffrn_orient_matrix_UB_33      -0.0297882000
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80513
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.524
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       needle
_exptl_crystal_F_000             3462
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1687
_refine_ls_number_reflns         30441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17677
_reflns_number_total             30441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03880a1.cif
_cod_data_source_block           Fe1
_cod_original_formula_sum        'C59 H63 Cl2 F4 Fe N4 O4.50'
_cod_database_code               7701829
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 89.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.45
_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:
 C01F(H01F), C020(H020), C29(H29), C16A(H16A), C29A(H29A), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C14B(H14B), C14A(H14A), C12B(H12B), C6(H6), C12A(H12A), C01V(H01V),
 C01X(H01X), C5(H5), C4B(H4B), C18A(H18A), C12(H12), C22(H22), C14(H14),
 C31(H31), C02N(H02N), C21(H21), C35(H35), C02T(H02T), C41A(H41A), C5A(H5A),
 C02W(H02W), C6A(H6A), C46(H46), C032(H032), C44(H44), C32(H32), C037(H037),
 C039(H039), C5B(H5B), C4A(H4A), C22A(H22A), C03F(H03F), C46A(H46A), C45A(H45A),
  C19A(H19A), C6B(H6B), C34(H34), C45(H45), C24(H24), C44A(H44A), C37A(H37A),
 C041(H041), C37(H37), C35A(H35A), C21A(H21A), C25(H25), C34A(H34A), C24A(H24A),
  C04B(H04B), C28A(H28A), C41(H41), C04E(H04E), C28(H28), C19(H19), C04H(H04H),
 C18(H18), C04J(H04J), C44B(H44B), C04Q(H04Q), C38A(H38A), C40A(H40A),
 C25A(H25A), C38(H38), C27(H27), C40(H40), C050(H050), C27A(H27A), C45B(H45B),
 C46B(H46B), C31A(H31A), C32A(H32A)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C1B(H1BA,H1BB,H1BC), C9A(H9AA,H9AB,H9AC), C1(H1A,H1B,H1C),
 C48(H48G,H48H,H48I), C9B(H9BA,H9BB,H9BC), C49A(H49A,H49B,H49C), C03U(H03A,H03B,
 H03C), C48A(H48A,H48B,H48C), C49(H49G,H49H,H49I), C49B(H49D,H49E,H49F),
 C48B(H48D,H48E,H48F)
;
_shelx_res_checksum              66252
_shelx_fab_checksum              8153
_platon_squeeze_special_details
;
A solvent mask was calculated and 630 electrons were
found in a volume of 2857\%A^3 in 1 void per unit cell.
This is consistent with the presence of 2.5[C4H10O] per
Formula Unit which account for 630 electrons per unit cell.
;
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.781