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#$Date: 2021-01-05 09:21:11 +0200 (Tue, 05 Jan 2021) $
#$Revision: 260509 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706249.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_7706249
loop_
_publ_author_name
'Papanikolaou, Michael G.'
'Elliott, Alexander'
'McAllister, James'
'Gallos, John K.'
'Keramidas, Anastasios D.'
'Kabanos, Themistoklis A.'
'Sproules, Stephen'
'Miras, Haralampos N.'
_publ_section_title
;
 Electrocatalytic hydrogen production by dinuclear cobalt(II) compounds
 containing redox-active diamidate ligands: a combined experimental and
 theoretical study.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15718
_journal_page_last               15730
_journal_paper_doi               10.1039/d0dt02617d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H30 Co2 N10 O4, 2(C HCl3) [+ solvent]'
_chemical_formula_sum            'C52 H32 Cl6 Co2 N10 O4'
_chemical_formula_weight         1191.43
_space_group_crystal_system      hexagonal
_space_group_IT_number           172
_space_group_name_Hall           'P 64'
_space_group_name_H-M_alt        'P 64'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-13 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.412(3)
_cell_length_b                   18.412(3)
_cell_length_c                   13.362(3)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.679
_cell_measurement_theta_min      2.210
_cell_volume                     3922.9(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.1471
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33616
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.989
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.6402
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             1806
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0163P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                3181
_reflns_number_total             5245
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02617d2.cif
_cod_data_source_block           Compound_1
_cod_original_cell_volume        3922.8(18)
_cod_database_code               7706249
_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   0.826
_shelx_estimated_absorpt_t_max   0.916
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z'
'y, -x+y, z+1/3'
'x-y, x, z+2/3'
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
C1 C 0.4823(4) 0.2653(4) 0.4625(5) 0.0263(17) Uani 1 1 d . . . . .
H1 H 0.484642 0.259372 0.532824 0.032 Uiso 1 1 calc R U . . .
C2 C 0.5053(4) 0.2192(4) 0.3997(5) 0.0268(17) Uani 1 1 d . . . . .
H2 H 0.522804 0.182782 0.426988 0.032 Uiso 1 1 calc R U . . .
C3 C 0.5020(4) 0.2274(4) 0.2991(5) 0.0274(17) Uani 1 1 d . . . . .
H3 H 0.517691 0.196585 0.255902 0.033 Uiso 1 1 calc R U . . .
C4 C 0.4760(4) 0.2801(4) 0.2583(5) 0.0234(16) Uani 1 1 d . . . . .
C5 C 0.4537(4) 0.3249(4) 0.3259(4) 0.0179(15) Uani 1 1 d . . . . .
C6 C 0.4288(4) 0.3826(4) 0.2924(5) 0.0227(17) Uani 1 1 d . . . . .
C7 C 0.4268(4) 0.3936(5) 0.1904(5) 0.0321(19) Uani 1 1 d . . . . .
H7 H 0.411711 0.432485 0.165180 0.039 Uiso 1 1 calc R U . . .
C8 C 0.4473(5) 0.3472(5) 0.1236(5) 0.036(2) Uani 1 1 d . . . . .
H6 H 0.444671 0.355038 0.053651 0.044 Uiso 1 1 calc R U . . .
C9 C 0.4704(4) 0.2923(5) 0.1552(5) 0.0327(19) Uani 1 1 d . . . . .
H5 H 0.482951 0.261667 0.107809 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3717(4) 0.4668(4) 0.3500(5) 0.0231(15) Uani 1 1 d . . . . .
C11 C 0.3627(4) 0.5084(4) 0.4421(4) 0.0213(16) Uani 1 1 d . . . . .
C12 C 0.2963(4) 0.5256(4) 0.4469(5) 0.0318(18) Uani 1 1 d . . . . .
H11 H 0.260623 0.515282 0.390916 0.038 Uiso 1 1 calc R U . . .
C13 C 0.2841(4) 0.5573(4) 0.5339(5) 0.0352(19) Uani 1 1 d . . . . .
H12 H 0.239669 0.569320 0.539337 0.042 Uiso 1 1 calc R U . . .
C14 C 0.3382(4) 0.5720(4) 0.6148(5) 0.0268(16) Uani 1 1 d . . . . .
H13 H 0.330765 0.593378 0.676264 0.032 Uiso 1 1 calc R U . . .
C15 C 0.4017(4) 0.5548(4) 0.6037(4) 0.0165(15) Uani 1 1 d . . . . .
C16 C 0.4636(4) 0.5766(4) 0.6885(5) 0.0221(16) Uani 1 1 d . . . . .
C17 C 0.3893(4) 0.3707(4) 0.7187(4) 0.0192(16) Uani 1 1 d . . . . .
C18 C 0.3901(4) 0.3686(4) 0.8247(5) 0.0296(18) Uani 1 1 d . . . . .
H17 H 0.441390 0.386494 0.859284 0.036 Uiso 1 1 calc R U . . .
C19 C 0.3147(5) 0.3398(5) 0.8789(5) 0.039(2) Uani 1 1 d . . . . .
H18 H 0.316340 0.341071 0.950016 0.047 Uiso 1 1 calc R U . . .
C20 C 0.2413(4) 0.3109(5) 0.8324(6) 0.0372(19) Uani 1 1 d . . . . .
H19 H 0.191360 0.289884 0.870790 0.045 Uiso 1 1 calc R U . . .
C21 C 0.2365(4) 0.3111(4) 0.7253(5) 0.0275(18) Uani 1 1 d . . . . .
C22 C 0.3118(4) 0.3401(4) 0.6706(5) 0.0212(15) Uani 1 1 d . . . . .
C23 C 0.1613(5) 0.2823(4) 0.6726(6) 0.0392(19) Uani 1 1 d . . . . .
H22 H 0.109676 0.261719 0.707380 0.047 Uiso 1 1 calc R U . . .
C24 C 0.1632(4) 0.2841(5) 0.5696(6) 0.041(2) Uani 1 1 d . . . . .
H23 H 0.113225 0.266050 0.532163 0.049 Uiso 1 1 calc R U . . .
C25 C 0.2401(4) 0.3132(4) 0.5213(5) 0.0302(18) Uani 1 1 d . . . . .
H24 H 0.240440 0.312025 0.450228 0.036 Uiso 1 1 calc R U . . .
C26 C 0.2046(5) 0.2825(5) 0.2158(5) 0.036(2) Uani 1 1 d . . . . .
H25 H 0.257707 0.337946 0.216359 0.044 Uiso 1 1 calc R U . . .
N1 N 0.4151(3) 0.5231(3) 0.5200(4) 0.0186(12) Uani 1 1 d . . . . .
N2 N 0.4107(3) 0.4232(3) 0.3687(3) 0.0172(13) Uani 1 1 d . . . . .
N3 N 0.4576(3) 0.3164(3) 0.4282(4) 0.0190(12) Uani 1 1 d . . . . .
N4 N 0.3121(3) 0.3420(3) 0.5685(4) 0.0216(13) Uani 1 1 d . . . . .
N5 N 0.4581(3) 0.3983(3) 0.6555(4) 0.0182(13) Uani 1 1 d . . . . .
O2 O 0.3413(3) 0.4741(3) 0.2697(3) 0.0337(12) Uani 1 1 d . . . . .
O3 O 0.4387(3) 0.5733(3) 0.7758(3) 0.0269(12) Uani 1 1 d . . . . .
Co1 Co 0.43414(5) 0.40213(6) 0.50921(6) 0.0206(2) Uani 1 1 d . . . . .
Cl1 Cl 0.12937(14) 0.29253(15) 0.28547(16) 0.0589(7) Uani 1 1 d . . . . .
Cl2 Cl 0.22520(16) 0.20938(16) 0.27123(18) 0.0697(7) Uani 1 1 d . . . . .
Cl3 Cl 0.17320(17) 0.25700(17) 0.09325(16) 0.0800(9) Uani 1 1 d . . . . .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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 C1 C2 122.9(6) . . ?
N3 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.8(7) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 121.1(7) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C9 125.0(6) . . ?
C3 C4 C5 117.3(6) . . ?
C9 C4 C5 117.7(6) . . ?
N3 C5 C4 121.2(6) . . ?
N3 C5 C6 116.7(5) . . ?
C4 C5 C6 122.1(6) . . ?
C7 C6 N2 127.5(6) . . ?
C7 C6 C5 117.5(6) . . ?
N2 C6 C5 115.0(5) . . ?
C6 C7 C8 120.1(7) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 122.4(7) . . ?
C9 C8 H6 118.8 . . ?
C7 C8 H6 118.8 . . ?
C8 C9 C4 120.2(6) . . ?
C8 C9 H5 119.9 . . ?
C4 C9 H5 119.9 . . ?
O2 C10 N2 128.9(6) . . ?
O2 C10 C11 118.7(6) . . ?
N2 C10 C11 112.4(6) . . ?
N1 C11 C12 122.2(6) . . ?
N1 C11 C10 118.9(6) . . ?
C12 C11 C10 118.8(6) . . ?
C13 C12 C11 118.7(6) . . ?
C13 C12 H11 120.6 . . ?
C11 C12 H11 120.6 . . ?
C12 C13 C14 118.9(6) . . ?
C12 C13 H12 120.5 . . ?
C14 C13 H12 120.5 . . ?
C15 C14 C13 118.8(6) . . ?
C15 C14 H13 120.6 . . ?
C13 C14 H13 120.6 . . ?
N1 C15 C14 124.0(6) . . ?
N1 C15 C16 117.5(5) . . ?
C14 C15 C16 118.5(6) . . ?
O3 C16 N5 128.9(6) . 4_665 ?
O3 C16 C15 118.7(6) . . ?
N5 C16 C15 112.4(6) 4_665 . ?
N5 C17 C22 115.3(5) . . ?
N5 C17 C18 126.7(6) . . ?
C22 C17 C18 118.0(6) . . ?
C19 C18 C17 120.1(7) . . ?
C19 C18 H17 120.0 . . ?
C17 C18 H17 120.0 . . ?
C20 C19 C18 121.3(7) . . ?
C20 C19 H18 119.3 . . ?
C18 C19 H18 119.3 . . ?
C19 C20 C21 121.1(7) . . ?
C19 C20 H19 119.5 . . ?
C21 C20 H19 119.5 . . ?
C23 C21 C22 118.7(6) . . ?
C23 C21 C20 123.5(7) . . ?
C22 C21 C20 117.8(7) . . ?
N4 C22 C17 117.2(6) . . ?
N4 C22 C21 121.1(6) . . ?
C17 C22 C21 121.6(6) . . ?
C24 C23 C21 119.0(7) . . ?
C24 C23 H22 120.5 . . ?
C21 C23 H22 120.5 . . ?
C23 C24 C25 118.7(7) . . ?
C23 C24 H23 120.6 . . ?
C25 C24 H23 120.6 . . ?
N4 C25 C24 123.8(7) . . ?
N4 C25 H24 118.1 . . ?
C24 C25 H24 118.1 . . ?
Cl3 C26 Cl2 111.6(4) . . ?
Cl3 C26 Cl1 110.9(4) . . ?
Cl2 C26 Cl1 110.2(4) . . ?
Cl3 C26 H25 108.0 . . ?
Cl2 C26 H25 108.0 . . ?
Cl1 C26 H25 108.0 . . ?
C15 N1 C11 117.4(5) . . ?
C15 N1 Co1 102.2(4) . 4_665 ?
C11 N1 Co1 124.9(4) . 4_665 ?
C15 N1 Co1 126.3(4) . . ?
C11 N1 Co1 100.8(4) . . ?
Co1 N1 Co1 82.35(15) 4_665 . ?
C10 N2 C6 121.8(5) . . ?
C10 N2 Co1 121.4(4) . . ?
C6 N2 Co1 116.5(4) . . ?
C1 N3 C5 118.8(6) . . ?
C1 N3 Co1 128.7(4) . . ?
C5 N3 Co1 112.2(4) . . ?
C25 N4 C22 118.5(6) . . ?
C25 N4 Co1 128.9(5) . . ?
C22 N4 Co1 112.4(4) . . ?
C16 N5 C17 123.3(6) 4_665 . ?
C16 N5 Co1 121.4(4) 4_665 . ?
C17 N5 Co1 115.3(4) . . ?
N2 Co1 N5 170.8(2) . . ?
N2 Co1 N4 100.2(2) . . ?
N5 Co1 N4 79.1(2) . . ?
N2 Co1 N3 79.1(2) . . ?
N5 Co1 N3 109.78(19) . . ?
N4 Co1 N3 111.18(19) . . ?
N2 Co1 N1 104.09(19) . 4_665 ?
N5 Co1 N1 75.63(19) . 4_665 ?
N4 Co1 N1 154.40(19) . 4_665 ?
N3 Co1 N1 81.42(17) . 4_665 ?
N2 Co1 N1 74.57(19) . . ?
N5 Co1 N1 96.29(19) . . ?
N4 Co1 N1 81.61(18) . . ?
N3 Co1 N1 152.50(18) . . ?
N1 Co1 N1 97.24(15) 4_665 . ?
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
C1 N3 1.315(7) . ?
C1 C2 1.401(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.356(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(9) . ?
C3 H3 0.9500 . ?
C4 C9 1.408(9) . ?
C4 C5 1.416(8) . ?
C5 N3 1.383(7) . ?
C5 C6 1.423(8) . ?
C6 C7 1.382(9) . ?
C6 N2 1.400(8) . ?
C7 C8 1.411(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.347(9) . ?
C8 H6 0.9500 . ?
C9 H5 0.9500 . ?
C10 O2 1.248(7) . ?
C10 N2 1.340(7) . ?
C10 C11 1.502(8) . ?
C11 N1 1.351(7) . ?
C11 C12 1.409(9) . ?
C12 C13 1.369(8) . ?
C12 H11 0.9500 . ?
C13 C14 1.403(9) . ?
C13 H12 0.9500 . ?
C14 C15 1.362(8) . ?
C14 H13 0.9500 . ?
C15 N1 1.341(7) . ?
C15 C16 1.512(8) . ?
C16 O3 1.244(7) . ?
C16 N5 1.350(7) 4_665 ?
C17 N5 1.390(8) . ?
C17 C22 1.401(8) . ?
C17 C18 1.417(8) . ?
C18 C19 1.414(9) . ?
C18 H17 0.9500 . ?
C19 C20 1.333(9) . ?
C19 H18 0.9500 . ?
C20 C21 1.434(9) . ?
C20 H19 0.9500 . ?
C21 C23 1.400(10) . ?
C21 C22 1.415(9) . ?
C22 N4 1.364(8) . ?
C23 C24 1.376(9) . ?
C23 H22 0.9500 . ?
C24 C25 1.396(9) . ?
C24 H23 0.9500 . ?
C25 N4 1.318(7) . ?
C25 H24 0.9500 . ?
C26 Cl3 1.722(7) . ?
C26 Cl2 1.735(7) . ?
C26 Cl1 1.754(7) . ?
C26 H25 1.0000 . ?
N1 Co1 2.408(5) 4_665 ?
N1 Co1 2.426(5) . ?
N2 Co1 2.007(5) . ?
N3 Co1 2.128(5) . ?
N4 Co1 2.101(5) . ?
N5 Co1 2.012(5) . ?
