Synthesis of characteristic polyisoprenes using rationally designed iminopyridyl metal (Fe and Co) precatalysts: investigation of co-catalysts and steric influence on their catalytic activity
Lin, Wenhua; Zhang, Liping; Suo, Hongyi; Vignesh, Arumugam; Yousuf, Nighat; Hao, Xiang; Sun, Wen-Hua; New Journal of Chemistry 44 (2020) 8076–8084; doi:10.1039/D0NJ00942C

data_7059515
_publ_section_title
;
 Synthesis of characteristic polyisoprenes using rationally designed
 iminopyridyl metal (Fe and Co) precatalysts: investigation of
 co-catalysts and steric influence on their catalytic activity
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8076
_journal_page_last               8084
_journal_paper_doi               10.1039/D0NJ00942C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C34 H28 Cl4 Fe2 N4 O, C H2 Cl2'
_chemical_formula_sum            'C35 H30 Cl6 Fe2 N4 O'
_chemical_formula_weight         847.03
_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     iterative
_audit_creation_date             2019-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.360(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0681(3)
_cell_length_b                   22.9447(9)
_cell_length_c                   21.9040(8)
_cell_measurement_reflns_used    7732
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      25.7590
_cell_measurement_theta_min      3.5300
_cell_volume                     4037.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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    -60.00 -32.64   0.38   14.00    --    5.00  45.00 165.63   72
  2  \w    -83.00 -49.94   0.38   14.00    --  -14.80  45.00  30.00   87
  3  \w   -103.00 -63.86   0.38   14.00    --  -14.80  45.00 171.06  103
  4  \w   -104.00 -68.66   0.38   14.00    --  -14.80  45.00 150.00   93
  5  \w    -33.00  70.36   0.38   14.00    --  -14.80  45.00 150.00  272
  6  \w    -55.00  72.30   0.38   14.00    --  -14.80  45.00 -19.91  335
  7  \w    -34.00  73.16   0.38   14.00    --  -14.80  45.00  30.00  282
  8  \w     47.00  73.22   0.38   14.00    --  -14.80  45.00 171.06   69
  9  \w     18.00  44.22   0.38   14.00    --  -14.80  45.00 120.00   69
 10  \w    -94.00 -48.78   0.38   14.00    --  -14.80  45.00  90.00  119
 11  \w    -16.00  72.16   0.38   14.00    --  -14.80  45.00  90.00  232
 12  \w    -56.00 -29.78   0.38   14.00    --  -14.80  45.00 120.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0679487000
_diffrn_orient_matrix_UB_12      -0.0167389000
_diffrn_orient_matrix_UB_13      -0.0133885000
_diffrn_orient_matrix_UB_21      0.0538546000
_diffrn_orient_matrix_UB_22      -0.0241164000
_diffrn_orient_matrix_UB_23      -0.0025780000
_diffrn_orient_matrix_UB_31      -0.0170527000
_diffrn_orient_matrix_UB_32      -0.0096858000
_diffrn_orient_matrix_UB_33      0.0295029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            9241
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.575
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1293P)^2^+5.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6420
_reflns_number_total             9241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00942c2.cif
_cod_data_source_block           Fe1
_cod_depositor_comments
;Adding full bibliography for 7059515--7059517.cif.

 Adding full bibliography for 7059515--7059517.cif.
;
_cod_database_code               7059515
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNClFe
_chemical_oxdiff_usercomment     'C H N Fe Cl'
_reflns_odcompleteness_completeness 95.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5741(19)
 0.4259(19)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C13(H13), C4(H4), C17(H17), C11(H11), C16(H16), C28(H28),
 C2(H2), C15(H15), C34(H34), C12(H12), C27(H27), C33(H33), C21(H21), C3(H3),
 C18(H18), C32(H32), C29(H29), C20(H20), C30(H30), C19(H19)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              44270
_shelx_fab_checksum              17798
_platon_squeeze_void_probe_radius 1.20
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.761