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_7059517
_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         '2(C25 H22 Cl2 Co N2)'
_chemical_formula_sum            'C50 H0.5 Cl4 Co2 N4'
_chemical_formula_weight         916.70
_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     iterative
_audit_creation_date             2019-04-15
_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                88.106(2)
_cell_angle_beta                 88.243(2)
_cell_angle_gamma                85.866(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9259(2)
_cell_length_b                   13.5150(3)
_cell_length_c                   19.0721(5)
_cell_measurement_reflns_used    13090
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      28.9440
_cell_measurement_theta_min      3.5180
_cell_volume                     2292.57(9)
_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 0.879
_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 -35.00   0.50   10.00    --    5.00  45.00 171.70   52
  2  \w   -103.00 -12.00   0.50   10.00    --  -14.80  45.00 165.68  182
  3  \w    -32.00  -6.00   0.50   10.00    --  -14.80  45.00  90.00   52
  4  \w     -1.00  27.00   0.50   10.00    --  -14.80  45.00  60.00   56
  5  \w   -104.00  74.00   0.50   10.00    --  -14.80  45.00 120.00  356
  6  \w    -84.00 -59.00   0.50   10.00    --  -14.80  45.00  90.00   50
  7  \w    -86.00 -60.00   0.50   10.00    --  -14.80  45.00  60.00   52
  8  \w      1.00  27.00   0.50   10.00    --  -14.80  45.00  90.00   52
  9  \w      4.00  74.00   0.50   10.00    --  -14.80  45.00 -15.95  140
 10  \w    -19.00  57.00   0.50   10.00    --  -14.80  45.00  30.00  152
 11  \w    -55.00  73.00   0.50   10.00    --  -14.80  45.00 179.14  256
;
_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      0.0751037000
_diffrn_orient_matrix_UB_12      -0.0110416000
_diffrn_orient_matrix_UB_13      0.0104396000
_diffrn_orient_matrix_UB_21      0.0173695000
_diffrn_orient_matrix_UB_22      -0.0231028000
_diffrn_orient_matrix_UB_23      -0.0323933000
_diffrn_orient_matrix_UB_31      0.0202617000
_diffrn_orient_matrix_UB_32      0.0459978000
_diffrn_orient_matrix_UB_33      -0.0150814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42040
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.717
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89398
_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    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             901
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0358P)^2^+0.2758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9018
_reflns_number_total             12534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00942c2.cif
_cod_data_source_block           Co3
_cod_depositor_comments
;Adding full bibliography for 7059515--7059517.cif.

 Adding full bibliography for 7059515--7059517.cif.
;
_cod_original_formula_sum        'C50 H0.50 Cl4 Co2 N4'
_cod_database_code               7059517
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C N H Co Cl'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
;
_shelx_res_checksum              28898
_shelx_fab_checksum              75903
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.833