Polymerisation of styrene using pincer type amine functionalized azo aromatic complexes of Co(II) as catalysts.
Goswami, Bappaditya; Khatua, Manas; Samanta, Subhas; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1454–1463; doi:10.1039/d1dt02622d

data_7709092
_publ_section_title
;
 Polymerisation of styrene using pincer type amine functionalized azo
 aromatic complexes of Co(II) as catalysts.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1454
_journal_page_last               1463
_journal_paper_doi               10.1039/d1dt02622d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C20 H20 Cl2 Co N4'
_chemical_formula_sum            'C20 H20 Cl2 Co N4'
_chemical_formula_weight         446.23
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-05-14 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.053(5)
_cell_angle_beta                 75.080(5)
_cell_angle_gamma                71.225(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1251(6)
_cell_length_b                   9.7997(6)
_cell_length_c                   11.9466(6)
_cell_measurement_reflns_used    3650
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      66.0600
_cell_measurement_theta_min      3.7840
_cell_volume                     975.96(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 97-2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_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    -29.00  63.00   1.00    1.00    --   26.33  38.00  28.00   92
  2  \w     81.00 107.00   1.00    1.00    --   26.33  38.00  28.00   26
  3  \w     58.00  96.00   1.00    1.00    --   26.33  57.00  90.00   38
  4  \w    104.00 150.00   1.00    2.00    --   67.17 111.00 150.00   46
  5  \w    139.00 165.00   1.00    2.00    --  108.00 138.00 120.00   26
  6  \w    119.00 177.00   1.00    2.00    --  108.00 138.00  30.00   58
  7  \w    147.00 173.00   1.00    2.00    --  108.00 138.00 -60.00   26
  8  \w    143.00 176.00   1.00    2.00    --  108.00 104.00 -60.00   33
  9  \w    110.00 149.00   1.00    2.00    --   67.17 178.00 -90.00   39
 10  \w    102.00 128.00   1.00    2.00    --  108.00 138.00 -60.00   26
 11  \w    102.00 148.00   1.00    2.00    --  108.00 104.00 -90.00   46
 12  \w    105.00 152.00   1.00    2.00    --   67.17 111.00-120.00   47
 13  \w    102.00 128.00   1.00    2.00    --   67.17 111.00 -90.00   26
 14  \w    102.00 176.00   1.00    2.00    --  108.00 104.00   0.00   74
 15  \w    103.00 143.00   1.00    2.00    --   67.17 111.00 120.00   40
 16  \w    100.00 144.00   1.00    2.00    --   67.17 111.00  60.00   44
 17  \w     82.00 120.00   1.00    1.00    --   26.33 178.00 -60.00   38
 18  \w     57.00  83.00   1.00    2.00    --   67.17 178.00 -90.00   26
 19  \w     -8.00  18.00   1.00    1.00    --   26.33  57.00  90.00   26
 20  \w     27.00  53.00   1.00    1.00    --   26.33  57.00  90.00   26
 21  \w    -24.00 157.00   1.00    2.00    --   67.17   0.00 -60.00  181
 22  \w    125.00 176.00   1.00    2.00    --  108.00 -32.00 -90.00   51
 23  \w    134.00 160.00   1.00    2.00    --  108.00 -11.00 -30.00   26
 24  \w     90.00 137.00   1.00    2.00    --  108.00 -54.00  30.00   47
 25  \w     77.00 103.00   1.00    2.00    --  108.00 -89.00  90.00   26
 26  \w     53.00  79.00   1.00    2.00    --  108.00 -54.00  30.00   26
 27  \w     46.00 138.00   1.00    2.00    --  108.00 -65.00  30.00   92
 28  \w     73.00 111.00   1.00    2.00    --  108.00-104.00 -60.00   38
 29  \w     84.00 110.00   1.00    2.00    --   67.17-111.00-150.00   26
 30  \w     76.00 102.00   1.00    2.00    --   67.17 -61.00-150.00   26
 31  \w     60.00  86.00   1.00    2.00    --  108.00 -54.00-180.00   26
 32  \w     31.00  65.00   1.00    2.00    --  108.00 -32.00 -90.00   34
 33  \w     31.00 133.00   1.00    2.00    --  108.00 -65.00 -90.00  102
 34  \w     64.00  98.00   1.00    2.00    --  108.00  21.00  60.00   34
 35  \w     58.00 143.00   1.00    2.00    --  108.00  43.00  90.00   85
 36  \w     82.00 133.00   1.00    2.00    --  108.00  77.00  90.00   51
 37  \w     63.00 158.00   1.00    2.00    --  108.00  43.00  30.00   95
 38  \w     43.00 113.00   1.00    2.00    --  108.00-104.00  60.00   70
 39  \w     30.00 122.00   1.00    2.00    --  108.00-132.00 -99.75   92
 40  \w     14.00  80.00   1.00    2.00    --   67.17-111.00-150.00   66
 41  \w     -7.00  51.00   1.00    2.00    --   67.17 -61.00-150.00   58
 42  \w     37.00 177.00   1.00    2.00    --  108.00  32.00 -30.00  140
 43  \w      9.00  98.00   1.00    1.00    --   26.33  57.00-150.00   89
 44  \w     10.00  50.00   1.00    2.00    --   67.17 -61.00  30.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0593954000
_diffrn_orient_matrix_UB_12      0.1602014000
_diffrn_orient_matrix_UB_13      0.0417389000
_diffrn_orient_matrix_UB_21      0.1709092000
_diffrn_orient_matrix_UB_22      0.0069576000
_diffrn_orient_matrix_UB_23      -0.0485672000
_diffrn_orient_matrix_UB_31      -0.0370702000
_diffrn_orient_matrix_UB_32      0.0439964000
_diffrn_orient_matrix_UB_33      -0.1173033000
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6384
_diffrn_reflns_theta_full        66.20
_diffrn_reflns_theta_max         66.20
_diffrn_reflns_theta_min         3.83
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.367
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1897P)^2^+1.1085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2411
_refine_ls_wR_factor_ref         0.2543
_reflns_number_gt                2977
_reflns_number_total             3396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt02622d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7709090--7709093.cif.'
_cod_original_cell_volume        975.96(10)
_cod_database_code               7709092
_chemical_oxdiff_formula         'C H N Co Cl'
_reflns_odcompleteness_completeness 97.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C9(H9), C5(H5), C17(H17), C3(H3), C16(H16), C8(H8),
 C4(H4a), C2(H2), C1(H1)
2.d Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C19(H19a,H19b,H19c)
;
_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 4.163
_oxdiff_exptl_absorpt_empirical_full_min 0.376