#------------------------------------------------------------------------------
#$Date: 2020-07-06 06:08:05 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253898 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/36/7703690.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7703690
loop_
_publ_author_name
'Sinha, Suman'
'Das, Siuli'
'Mondal, Rakesh'
'Mandal, Sutanuva'
'Paul, Nanda D.'
_publ_section_title
;
 Cobalt complexes of redox noninnocent azo-aromatic pincers. Isolation,
 characterization, and application as catalysts for the synthesis of
 quinazolin-4(3H)-ones.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8448
_journal_page_last               8459
_journal_paper_doi               10.1039/d0dt00394h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C24 H16 Cl2 Co N6'
_chemical_formula_weight         518.26
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.699(2)
_cell_angle_beta                 98.267(2)
_cell_angle_gamma                90.736(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4667(7)
_cell_length_b                   10.9982(9)
_cell_length_c                   12.1179(10)
_cell_measurement_reflns_used    438
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.99
_cell_volume                     1092.45(16)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      127(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31435
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.163
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6270
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       Rod
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0324
_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/[σ²(Fo²)+(0.0311P)²+1.0058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4039
_reflns_number_total             4840
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00394h2.cif
_cod_data_source_block           2_0m
_cod_depositor_comments
'Adding full bibliography for 7703688--7703690.cif.'
_cod_database_code               7703690
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.627
_shelx_estimated_absorpt_t_max   0.746
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.72272(4) 0.78750(3) 0.67111(2) 0.02093(9) Uani 0.95 1 d . . P A 1
CoA Co 0.7749(8) 0.7044(9) 0.6579(6) 0.0382(17) Uani 0.05 1 d . . P A 2
Cl1 Cl 0.72540(6) 0.71522(5) 0.83201(4) 0.02220(12) Uani 1 1 d . . . . .
Cl2 Cl 0.95591(6) 0.86333(5) 0.63690(5) 0.02648(13) Uani 1 1 d . . . . .
N1 N 0.6151(2) 0.96556(16) 0.75066(14) 0.0199(4) Uani 1 1 d . . . . .
N2 N 0.4788(2) 0.99194(16) 0.70604(15) 0.0216(4) Uani 1 1 d . . . . .
N3 N 0.5219(2) 0.81777(15) 0.56880(14) 0.0183(3) Uani 1 1 d . . . . .
N4 N 0.6887(2) 0.61988(15) 0.52614(14) 0.0186(3) Uani 1 1 d . . . . .
N5 N 0.8767(2) 0.50595(16) 0.60969(15) 0.0233(4) Uani 1 1 d . . . . .
N6 N 0.9305(2) 0.40000(17) 0.59928(15) 0.0240(4) Uani 1 1 d . . . . .
C1 C 0.6713(3) 1.04346(19) 0.85962(18) 0.0234(4) Uani 1 1 d . . . . .
C2 C 0.5690(3) 1.1022(2) 0.9303(2) 0.0311(5) Uani 1 1 d . . . . .
H2 H 0.456596 1.091056 0.908314 0.037 Uiso 1 1 calc R U . . .
C3 C 0.6323(3) 1.1777(3) 1.0341(2) 0.0421(6) Uani 1 1 d . . . . .
H3 H 0.562991 1.217469 1.084023 0.051 Uiso 1 1 calc R U . . .
C4 C 0.7964(3) 1.1952(2) 1.0651(2) 0.0404(6) Uani 1 1 d . . . . .
H4 H 0.839270 1.247120 1.136047 0.049 Uiso 1 1 calc R U . . .
C5 C 0.8974(3) 1.1376(2) 0.9933(2) 0.0347(6) Uani 1 1 d . . . . .
H5 H 1.009710 1.151616 1.013693 0.042 Uiso 1 1 calc R U . . .
C6 C 0.8351(3) 1.0591(2) 0.89129(19) 0.0285(5) Uani 1 1 d . . . . .
H6 H 0.904677 1.016244 0.843242 0.034 Uiso 1 1 calc R U . . .
C7 C 0.4327(2) 0.91504(18) 0.59795(17) 0.0198(4) Uani 1 1 d . . . . .
C8 C 0.3025(2) 0.94374(19) 0.52438(19) 0.0233(4) Uani 1 1 d . . . . .
H8 H 0.237543 1.010688 0.549135 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2700(2) 0.87388(19) 0.41623(19) 0.0227(4) Uani 1 1 d . . . . .
H9 H 0.184380 0.894078 0.364168 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3635(2) 0.77176(18) 0.38176(17) 0.0194(4) Uani 1 1 d . . . . .
C11 C 0.4856(2) 0.74564(18) 0.46333(16) 0.0173(4) Uani 1 1 d . . . . .
C12 C 0.3404(2) 0.69234(19) 0.27115(17) 0.0212(4) Uani 1 1 d . . . . .
H12 H 0.263010 0.711461 0.212921 0.025 Uiso 1 1 calc R U . . .
C13 C 0.4273(2) 0.5903(2) 0.24822(17) 0.0217(4) Uani 1 1 d . . . . .
H13 H 0.409005 0.538906 0.174071 0.026 Uiso 1 1 calc R U . . .
C14 C 0.5459(2) 0.55772(18) 0.33256(17) 0.0188(4) Uani 1 1 d . . . . .
C15 C 0.5777(2) 0.63800(18) 0.43983(16) 0.0171(4) Uani 1 1 d . . . . .
C16 C 0.6351(2) 0.44972(19) 0.31765(18) 0.0224(4) Uani 1 1 d . . . . .
H16 H 0.620170 0.392324 0.246571 0.027 Uiso 1 1 calc R U . . .
C17 C 0.7435(2) 0.42806(19) 0.40630(19) 0.0227(4) Uani 1 1 d . . . . .
H17 H 0.801852 0.354385 0.398020 0.027 Uiso 1 1 calc R U . . .
C18 C 0.7673(2) 0.51618(19) 0.50971(17) 0.0202(4) Uani 1 1 d . . . . .
C19 C 1.0323(3) 0.3812(2) 0.69850(18) 0.0244(4) Uani 1 1 d . . . . .
C20 C 1.0477(3) 0.4627(2) 0.8045(2) 0.0292(5) Uani 1 1 d . . . . .
H20 H 0.991576 0.537464 0.814084 0.035 Uiso 1 1 calc R U . . .
C21 C 1.1467(3) 0.4321(3) 0.8951(2) 0.0354(6) Uani 1 1 d . . . . .
H21 H 1.158536 0.485788 0.968163 0.043 Uiso 1 1 calc R U . . .
C22 C 1.2285(3) 0.3231(3) 0.8793(2) 0.0376(6) Uani 1 1 d . . . . .
H22 H 1.297130 0.302935 0.941606 0.045 Uiso 1 1 calc R U . . .
C23 C 1.2115(3) 0.2433(2) 0.7741(2) 0.0352(6) Uani 1 1 d . . . . .
H23 H 1.268298 0.168867 0.764240 0.042 Uiso 1 1 calc R U . . .
C24 C 1.1120(3) 0.2719(2) 0.6836(2) 0.0284(5) Uani 1 1 d . . . . .
H24 H 1.098267 0.216708 0.611307 0.034 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co Cl1 124.60(5) . . ?
N3 Co N1 70.24(6) . . ?
Cl1 Co N1 90.84(5) . . ?
N3 Co Cl2 116.83(5) . . ?
Cl1 Co Cl2 117.65(2) . . ?
N1 Co Cl2 100.50(5) . . ?
N3 Co N4 74.95(6) . . ?
Cl1 Co N4 106.45(5) . . ?
N1 Co N4 145.02(6) . . ?
Cl2 Co N4 97.94(5) . . ?
N4 CoA Cl1 133.7(4) . . ?
N4 CoA Cl2 110.7(3) . . ?
Cl1 CoA Cl2 114.7(3) . . ?
N2 N1 C1 113.77(17) . . ?
N2 N1 Co 118.75(13) . . ?
C1 N1 Co 126.51(13) . . ?
N1 N2 C7 111.01(17) . . ?
C7 N3 C11 118.47(17) . . ?
C7 N3 Co 121.75(13) . . ?
C11 N3 Co 119.42(13) . . ?
C18 N4 C15 117.36(17) . . ?
C18 N4 CoA 105.6(3) . . ?
C15 N4 CoA 136.8(3) . . ?
C18 N4 Co 130.82(14) . . ?
C15 N4 Co 111.52(13) . . ?
N6 N5 C18 110.74(18) . . ?
N5 N6 C19 113.58(18) . . ?
C2 C1 C6 120.7(2) . . ?
C2 C1 N1 122.5(2) . . ?
C6 C1 N1 116.84(19) . . ?
C1 C2 C3 119.2(2) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 119.8(2) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N3 C7 C8 122.55(18) . . ?
N3 C7 N2 117.02(18) . . ?
C8 C7 N2 120.38(18) . . ?
C9 C8 C7 118.86(19) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C8 C9 C10 120.1(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 117.01(19) . . ?
C11 C10 C12 118.09(18) . . ?
C9 C10 C12 124.89(19) . . ?
N3 C11 C10 122.86(18) . . ?
N3 C11 C15 115.93(17) . . ?
C10 C11 C15 121.20(18) . . ?
C13 C12 C10 120.92(19) . . ?
C13 C12 H12 119.5 . . ?
C10 C12 H12 119.5 . . ?
C12 C13 C14 121.78(19) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C16 116.17(18) . . ?
C15 C14 C13 118.49(18) . . ?
C16 C14 C13 125.34(19) . . ?
N4 C15 C14 124.60(18) . . ?
N4 C15 C11 116.08(17) . . ?
C14 C15 C11 119.30(18) . . ?
C17 C16 C14 119.62(19) . . ?
C17 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
C16 C17 C18 119.26(19) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
N4 C18 C17 122.91(19) . . ?
N4 C18 N5 111.70(17) . . ?
C17 C18 N5 125.38(19) . . ?
C24 C19 C20 121.4(2) . . ?
C24 C19 N6 114.6(2) . . ?
C20 C19 N6 124.0(2) . . ?
C21 C20 C19 118.5(2) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
C20 C21 C22 119.9(2) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.9(2) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 119.8(2) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C19 119.6(2) . . ?
C23 C24 H24 120.2 . . ?
C19 C24 H24 120.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N3 2.0284(17) . ?
Co Cl1 2.2473(6) . ?
Co N1 2.2643(17) . ?
Co Cl2 2.2580(6) . ?
Co N4 2.2573(17) . ?
CoA N4 1.730(7) . ?
CoA Cl1 2.190(7) . ?
CoA Cl2 2.386(8) . ?
N1 N2 1.266(2) . ?
N1 C1 1.433(3) . ?
N2 C7 1.407(3) . ?
N3 C7 1.336(3) . ?
N3 C11 1.352(2) . ?
N4 C18 1.322(3) . ?
N4 C15 1.350(3) . ?
N5 N6 1.246(2) . ?
N5 C18 1.440(3) . ?
N6 C19 1.428(3) . ?
C1 C2 1.380(3) . ?
C1 C6 1.384(3) . ?
C2 C3 1.389(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.397(3) . ?
C8 C9 1.366(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.411(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(3) . ?
C10 C12 1.429(3) . ?
C11 C15 1.429(3) . ?
C12 C13 1.353(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.429(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(3) . ?
C14 C16 1.410(3) . ?
C16 C17 1.371(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.407(3) . ?
C17 H17 0.9500 . ?
C19 C24 1.379(3) . ?
C19 C20 1.397(3) . ?
C20 C21 1.384(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
