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_7059516
_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         'C50 H44 Cl Fe N4, Cl4 Fe'
_chemical_formula_sum            'C50 H44 Cl5 Fe2 N4'
_chemical_formula_weight         989.84
_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             2020-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-06 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.766(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3261(6)
_cell_length_b                   11.7076(3)
_cell_length_c                   28.3441(10)
_cell_measurement_reflns_used    9425
_cell_measurement_temperature    170.00(12)
_cell_measurement_theta_max      72.4930
_cell_measurement_theta_min      2.6720
_cell_volume                     5505.1(3)
_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      170.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.951
_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     56.00  87.00   0.50    1.80    --   46.95  40.00  66.00   62
  2  \w     91.00 124.00   0.50    7.00    --  103.25  40.00  66.00   66
  3  \w     93.00 169.00   0.50    7.00    --  103.25  45.00  90.00  152
  4  \w     98.00 141.00   0.50    7.00    --  103.25  45.00 150.00   86
  5  \w     87.00 115.00   0.50    7.00    --  103.25 -45.00  60.00   56
  6  \w     50.00 117.00   0.50    7.00    --  103.25 -15.00  90.00  134
  7  \w     53.00 104.00   0.50    7.00    --  103.25 -94.00 120.00  102
  8  \w     44.00  82.00   0.50    7.00    --  103.25 -45.00  60.00   76
  9  \w     31.00 115.00   0.50    7.00    --  103.25 -40.00 -87.00  168
 10  \w     17.00  86.00   0.50    1.80    --   46.95-125.00-180.00  138
 11  \w    -10.00  39.00   0.50    1.80    --   46.95 -40.00 -87.00   98
 12  \w    -58.00  23.00   0.50    1.80    --  -46.95  40.00  66.00  162
 13  \w    -60.00 -35.00   0.50    7.00    --  -99.00  40.00  66.00   50
 14  \w   -116.00 -34.00   0.50    1.80    --  -46.95 -40.00 -87.00  164
 15  \w    -64.00 -37.00   0.50    7.00    --  -99.00  45.00 -90.00   54
 16  \w    -93.00 -67.00   0.50    7.00    --  -99.00  45.00 -90.00   52
 17  \w   -111.00 -66.00   0.50    7.00    --  -99.00  30.00-120.00   90
 18  \w   -118.00 -89.00   0.50    7.00    --  -99.00 -15.00-180.00   58
 19  \w   -146.00-103.00   0.50    7.00    --  -99.00 -40.00 -87.00   86
 20  \w   -167.00-120.00   0.50    7.00    --  -99.00 -15.00-180.00   94
;
_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      0.0527099000
_diffrn_orient_matrix_UB_12      -0.0647056000
_diffrn_orient_matrix_UB_13      0.0451463000
_diffrn_orient_matrix_UB_21      0.0731672000
_diffrn_orient_matrix_UB_22      0.0119330000
_diffrn_orient_matrix_UB_23      -0.0202177000
_diffrn_orient_matrix_UB_31      0.0223159000
_diffrn_orient_matrix_UB_32      0.1139511000
_diffrn_orient_matrix_UB_33      0.0278087000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35721
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.537
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30015
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       needle
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.033
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.1178
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3074
_refine_ls_wR_factor_ref         0.3179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7953
_reflns_number_total             10867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00942c2.cif
_cod_data_source_block           Fe3
_cod_depositor_comments
;Adding full bibliography for 7059515--7059517.cif.

 Adding full bibliography for 7059515--7059517.cif.
;
_cod_database_code               7059516
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N Fe Cl'
_reflns_odcompleteness_completeness 99.45
_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:
 C18(H18), C43(H43)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              51606
_shelx_fab_checksum              24875
_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 2.517
_oxdiff_exptl_absorpt_empirical_full_min 0.491