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_7709093
_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         'C19 Cl2 Co1 H21 N3 O2 '
_chemical_formula_sum            'C19 H21 Cl2 Co N3 O2'
_chemical_formula_weight         453.236
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-11-29 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.567(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4655(2)
_cell_length_b                   13.2728(2)
_cell_length_c                   16.6662(3)
_cell_measurement_reflns_used    27472
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      68.0210
_cell_measurement_theta_min      2.7370
_cell_volume                     2026.53(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9976
_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    -35.00  24.00   0.50    0.20    --   40.33 -12.00 -30.00  118
  2  \w    -30.00  31.00   0.50    0.20    --   40.33 -25.00-120.00  122
  3  \w     22.00 106.00   0.50    0.90    --   96.67 -96.00-180.00  168
  4  \w     44.00 127.00   0.50    0.90    --   96.67-145.00 -90.00  166
  5  \w     41.00  99.00   0.50    0.20    --   40.33-138.00  30.00  116
  6  \w     44.00 127.00   0.50    0.90    --   96.67-145.00  90.00  166
  7  \w     44.00 127.00   0.50    0.90    --   96.67-145.00 150.00  166
  8  \w     44.00 127.00   0.50    0.90    --   96.67-145.00   0.00  166
  9  \w     29.00  83.00   0.50    0.90    --   96.67 -68.00-180.00  108
 10  \w     29.00  83.00   0.50    0.90    --   96.67 -68.00 -90.00  108
 11  \w     30.00 109.00   0.50    0.90    --   96.67-117.00 -90.00  158
 12  \w     30.00  57.00   0.50    0.90    --   96.67 -50.00  30.00   54
 13  \w     29.00  68.00   0.50    0.90    --   96.67 -59.00  30.00   78
 14  \w     29.00  83.00   0.50    0.90    --   96.67 -68.00  90.00  108
 15  \w     30.00  57.00   0.50    0.90    --   96.67 -50.00 150.00   54
 16  \w     30.00  57.00   0.50    0.90    --   96.67 -50.00 120.00   54
 17  \w     22.00 106.00   0.50    0.90    --   96.67 -96.00  90.00  168
 18  \w     27.00 127.00   0.50    0.90    --   96.67 -87.00 -30.00  200
 19  \w     83.00 164.00   0.50    0.90    --   96.67  33.00 -30.00  162
 20  \w    106.00 169.00   0.50    0.90    --   96.67 102.00-101.00  126
 21  \w    105.00 170.00   0.50    0.90    --   96.67  96.00-120.00  130
 22  \w     83.00 164.00   0.50    0.90    --   96.67  33.00-120.00  162
 23  \w     80.00 163.00   0.50    0.90    --   96.67  42.00   0.00  166
 24  \w     83.00 164.00   0.50    0.90    --   96.67  33.00 150.00  162
 25  \w     83.00 164.00   0.50    0.90    --   96.67  33.00  60.00  162
 26  \w     83.00 164.00   0.50    0.90    --   96.67  33.00 -60.00  162
 27  \w     83.00 164.00   0.50    0.90    --   96.67  33.00-150.00  162
 28  \w     73.00 165.00   0.50    0.90    --   96.67  68.00 -30.00  184
 29  \w     75.00 164.00   0.50    0.90    --   96.67  59.00 120.00  178
 30  \w     75.00 164.00   0.50    0.90    --   96.67  59.00  60.00  178
 31  \w     73.00 165.00   0.50    0.90    --   96.67  68.00 150.00  184
 32  \w     75.00 164.00   0.50    0.90    --   96.67  59.00  90.00  178
 33  \w     70.00 165.00   0.50    0.90    --   96.67  77.00   0.00  190
 34  \w     73.00 165.00   0.50    0.90    --   96.67  68.00-120.00  184
 35  \w     70.00 165.00   0.50    0.90    --   96.67  77.00-180.00  190
 36  \w     29.00  68.00   0.50    0.90    --   96.67 -59.00 -30.00   78
 37  \w     29.00  83.00   0.50    0.90    --   96.67 -68.00   0.00  108
 38  \w     30.00 109.00   0.50    0.90    --   96.67-117.00 120.00  158
 39  \w     25.00 107.00   0.50    0.90    --   96.67-102.00 156.00  164
 40  \w      7.00  77.00   0.50    0.20    --   40.33-102.00 156.00  140
 41  \w    -30.00  31.00   0.50    0.20    --   40.33 -25.00  90.00  122
 42  \w     17.00 108.00   0.50    0.20    --   40.33  64.00  90.00  182
 43  \w     10.00  43.00   0.50    0.20    --   40.33  88.00  -1.37   66
 44  \w      9.00  43.00   0.50    0.20    --   40.33  90.00  24.23   68
 45  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 -30.00  190
 46  \w     17.00 108.00   0.50    0.20    --   40.33  64.00-150.00  182
 47  \w      9.00  43.00   0.50    0.20    --   40.33  90.00-163.06   68
 48  \w     12.00  43.00   0.50    0.20    --   40.33  81.00 -81.25   62
 49  \w      9.00  43.00   0.50    0.20    --   40.33  90.00 -85.55   68
 50  \w      7.00  35.00   0.50    0.20    --   40.33  94.00  30.16   56
 51  \w     14.00 109.00   0.50    0.20    --   40.33  77.00  90.00  190
 52  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 120.00  190
 53  \w     12.00  43.00   0.50    0.20    --   40.33  82.00 154.80   62
 54  \w     11.00  43.00   0.50    0.20    --   40.33  86.00 137.99   64
 55  \w    -43.00  26.00   0.50    0.20    --  -40.33  38.00 150.00  138
 56  \w    -24.00  35.00   0.50    0.20    --  -40.33  12.00 150.00  118
 57  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00  90.00  122
 58  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00 -60.00   64
 59  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00 -90.00   64
 60  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00-150.00  122
 61  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00 -90.00  122
 62  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00  30.00   64
 63  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00  60.00   64
 64  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00 120.00   64
 65  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00 150.00   64
 66  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00  90.00   64
 67  \w    -47.00 -15.00   0.50    0.90    --  -82.50  42.00   0.00   64
 68  \w    -63.00  27.00   0.50    0.20    --  -40.33  64.00  60.00  180
 69  \w    -77.00  15.00   0.50    0.20    --  -40.33 102.00-101.00  184
 70  \w    -35.00  24.00   0.50    0.20    --   40.33 -12.00-180.00  118
 71  \w     22.00 106.00   0.50    0.90    --   96.67 -96.00 -90.00  168
 72  \w    -81.00 -10.00   0.50    0.90    --  -82.50 102.00-101.00  142
 73  \w   -107.00 -21.00   0.50    0.20    --  -40.33 -50.00 -60.00  172
 74  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00 -90.00  182
 75  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00-180.00  182
 76  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00   0.00  182
 77  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00 150.00  182
 78  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00  60.00  182
 79  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 -90.00  192
 80  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00-150.00  192
 81  \w   -150.00 -69.00   0.50    0.90    --  -82.50 -33.00 120.00  162
 82  \w   -154.00 -84.00   0.50    0.90    --  -82.50-102.00 156.00  140
 83  \w   -151.00 -55.00   0.50    0.90    --  -82.50 -79.00  80.32  192
 84  \w   -153.00 -68.00   0.50    0.90    --  -82.50 -25.00   0.00  170
 85  \w   -151.00 -99.00   0.50    0.90    --  -82.50 -80.00 -27.24  104
 86  \w   -152.00 -55.00   0.50    0.90    --  -82.50 -78.00 -12.29  194
 87  \w   -152.00 -56.00   0.50    0.90    --  -82.50 -75.00 162.11  192
 88  \w   -152.00 -55.00   0.50    0.90    --  -82.50 -78.00 123.91  194
 89  \w   -152.00 -56.00   0.50    0.90    --  -82.50 -75.00 -57.88  192
 90  \w   -151.00 -55.00   0.50    0.90    --  -82.50 -77.00  30.00  192
 91  \w   -151.00 -55.00   0.50    0.90    --  -82.50 -77.00-136.19  192
 92  \w   -151.00 -54.00   0.50    0.90    --  -82.50 -80.00-161.29  194
 93  \w   -151.00 -54.00   0.50    0.90    --  -82.50 -80.00 -97.53  194
 94  \w   -151.00 -55.00   0.50    0.90    --  -82.50 -77.00  60.00  192
 95  \w   -151.00 -55.00   0.50    0.90    --  -82.50 -79.00 -72.57  192
 96  \w    -80.00  -9.00   0.50    0.90    --  -82.50  96.00 120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0459337000
_diffrn_orient_matrix_UB_12      -0.0178478000
_diffrn_orient_matrix_UB_13      -0.0812033000
_diffrn_orient_matrix_UB_21      -0.1553529000
_diffrn_orient_matrix_UB_22      -0.0368595000
_diffrn_orient_matrix_UB_23      -0.0420979000
_diffrn_orient_matrix_UB_31      -0.0450932000
_diffrn_orient_matrix_UB_32      0.1085912000
_diffrn_orient_matrix_UB_33      -0.0275921000
_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  0.1453
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50044
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9976
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.31
_diffrn_reflns_theta_min         4.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             928.544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.8770
_refine_diff_density_min         -1.0095
_refine_diff_density_rms         0.1409
_refine_ls_d_res_high            0.8297
_refine_ls_d_res_low             10.2491
_refine_ls_goodness_of_fit_ref   1.0351
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0351
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+4.4081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -7
_reflns_number_gt                3571
_reflns_number_total             3702
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt02622d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7709090--7709093.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_original_formula_sum        'C19 Cl2 Co1 H21 N3 O2 '
_cod_database_code               7709093
_chemical_oxdiff_formula         'C H N Cl Co'
_chemical_oxdiff_usercomment     LT
_reflns_odcompleteness_completeness 100.00
_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
2.a Ternary CH refined with riding coordinates:
 N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C19(H19), C10(H10), C1(H1), C15(H15), C18(H18),
 C2(H2), C5(H5), C17(H17), C3(H3a), C4(H4), C16(H16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 12.660
_oxdiff_exptl_absorpt_empirical_full_min 0.439