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#$Date: 2024-03-04 22:12:19 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290160 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/50/7715045.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_7715045
loop_
_publ_author_name
'Al-Shewiki, Rasha K'
'Weheabby, Saddam'
'Uhlig, Nell'
'Korb, Marcus'
'Pester, Tom'
'Zahn, Stefan'
'Grecchi, S.'
'Mussini, P. R.'
'Rüffer, Tobias'
'Lang, Heinrich'
_publ_section_title
;
 Cobalt(III)-containing penta-dentate "helmet"-type phthalogens:
 synthesis, solid-state structures and their thermal and electrochemical
 characterization.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3836
_journal_page_last               3854
_journal_paper_doi               10.1039/d3dt03950a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H16 Co N8'
_chemical_formula_sum            'C32 H16 Co N8'
_chemical_formula_weight         571.46
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.818(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5319(9)
_cell_length_b                   4.7748(3)
_cell_length_c                   17.1718(9)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    120
_cell_measurement_theta_max      65.8860
_cell_measurement_theta_min      4.6720
_cell_volume                     1146.38(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4539
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.352
_diffrn_reflns_theta_min         3.541
_exptl_absorpt_coefficient_mu    6.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         1977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0637P)²+0.0808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1708
_reflns_number_total             1977
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03950a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7715044--7715048.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7715045
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.668
_oxdiff_exptl_absorpt_empirical_full_max 2.087
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 -0.09105(19) 0.4281(6) -0.11923(17) 0.0225(6) Uani 1 1 d . . . . .
C2 C -0.0910(2) 0.5411(6) -0.19758(18) 0.0239(6) Uani 1 1 d . . . . .
C3 C -0.14705(19) 0.7462(6) -0.24557(17) 0.0265(6) Uani 1 1 d . . . . .
H3 H -0.1941 0.8410 -0.2287 0.032 Uiso 1 1 calc R U . . .
C4 C -0.1300(2) 0.8035(7) -0.31934(17) 0.0289(7) Uani 1 1 d . . . . .
H4 H -0.1656 0.9410 -0.3526 0.035 Uiso 1 1 calc R U . . .
C5 C -0.0597(2) 0.6571(7) -0.34451(17) 0.0288(7) Uani 1 1 d . . . . .
H5 H -0.0503 0.6976 -0.3948 0.035 Uiso 1 1 calc R U . . .
C6 C -0.0039(2) 0.4541(7) -0.29671(18) 0.0265(6) Uani 1 1 d . . . . .
H6 H 0.0434 0.3599 -0.3135 0.032 Uiso 1 1 calc R U . . .
C7 C -0.02109(19) 0.3958(6) -0.22258(17) 0.0238(6) Uani 1 1 d . . . . .
C8 C 0.02067(19) 0.1983(6) -0.15817(16) 0.0230(6) Uani 1 1 d . . . . .
C9 C 0.12762(19) -0.1516(6) -0.10216(16) 0.0218(6) Uani 1 1 d . . . . .
C10 C 0.20645(19) -0.3383(6) -0.10235(17) 0.0242(6) Uani 1 1 d . . . . .
C11 C 0.2626(2) -0.3715(6) -0.15596(17) 0.0273(6) Uani 1 1 d . . . . .
H11 H 0.2519 -0.2640 -0.2027 0.033 Uiso 1 1 calc R U . . .
C12 C 0.3349(2) -0.5707(7) -0.13707(19) 0.0298(7) Uani 1 1 d . . . . .
H12 H 0.3734 -0.5972 -0.1717 0.036 Uiso 1 1 calc R U . . .
C13 C 0.3507(2) -0.7320(7) -0.06678(18) 0.0297(7) Uani 1 1 d . . . . .
H13 H 0.3998 -0.8633 -0.0556 0.036 Uiso 1 1 calc R U . . .
C14 C 0.29532(19) -0.7019(6) -0.01330(17) 0.0268(6) Uani 1 1 d . . . . .
H14 H 0.3057 -0.8105 0.0333 0.032 Uiso 1 1 calc R U . . .
C15 C 0.2228(2) -0.4998(5) -0.03274(18) 0.0223(6) Uani 1 1 d . . . . .
C16 C 0.15377(19) -0.4086(6) 0.00924(16) 0.0234(6) Uani 1 1 d . . . . .
N1 N -0.02412(16) 0.2209(5) -0.09722(13) 0.0216(5) Uani 1 1 d . . . . .
N2 N 0.09185(16) 0.0273(5) -0.16093(14) 0.0222(5) Uani 1 1 d . . . . .
N3 N 0.09859(15) -0.1966(5) -0.03291(14) 0.0229(5) Uani 1 1 d . . . . .
N8 N -0.15052(17) 0.5223(5) -0.07871(15) 0.0240(6) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.0000 0.0000 0.0197(2) Uani 1 2 d S . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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'
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
N8 C1 N1 128.1(3) . . ?
N8 C1 C2 121.7(3) . . ?
N1 C1 C2 110.2(2) . . ?
C7 C2 C3 121.8(3) . . ?
C7 C2 C1 106.6(3) . . ?
C3 C2 C1 131.5(3) . . ?
C4 C3 C2 117.3(3) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C5 120.8(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 121.8(3) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C7 117.5(3) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 H6 121.3 . . ?
C6 C7 C2 120.7(3) . . ?
C6 C7 C8 133.2(3) . . ?
C2 C7 C8 106.1(2) . . ?
N2 C8 N1 127.4(3) . . ?
N2 C8 C7 122.6(2) . . ?
N1 C8 C7 110.0(2) . . ?
N2 C9 N3 127.7(2) . . ?
N2 C9 C10 122.9(2) . . ?
N3 C9 C10 109.4(2) . . ?
C15 C10 C11 120.8(3) . . ?
C15 C10 C9 106.8(2) . . ?
C11 C10 C9 132.4(3) . . ?
C12 C11 C10 117.7(3) . . ?
C12 C11 H11 121.1 . . ?
C10 C11 H11 121.1 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 121.9(3) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 116.7(3) . . ?
C13 C14 H14 121.7 . . ?
C15 C14 H14 121.7 . . ?
C10 C15 C14 122.0(3) . . ?
C10 C15 C16 106.4(2) . . ?
C14 C15 C16 131.7(3) . . ?
N8 C16 N3 128.3(3) 3 . ?
N8 C16 C15 121.6(3) 3 . ?
N3 C16 C15 110.1(2) . . ?
C1 N1 C8 107.1(2) . . ?
C1 N1 Co1 125.75(18) . . ?
C8 N1 Co1 127.13(19) . . ?
C9 N2 C8 121.3(2) . . ?
C16 N3 C9 107.3(2) . . ?
C16 N3 Co1 125.57(18) . . ?
C9 N3 Co1 127.12(19) . . ?
C16 N8 C1 121.5(3) 3 . ?
N3 Co1 N3 180.0 . 3 ?
N3 Co1 N1 89.24(9) . . ?
N3 Co1 N1 90.76(9) 3 . ?
N3 Co1 N1 90.76(9) . 3 ?
N3 Co1 N1 89.24(9) 3 3 ?
N1 Co1 N1 180.0 . 3 ?
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 N8 1.327(4) . ?
C1 N1 1.367(4) . ?
C1 C2 1.450(4) . ?
C2 C7 1.391(4) . ?
C2 C3 1.392(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.454(4) . ?
C8 N2 1.329(4) . ?
C8 N1 1.379(4) . ?
C9 N2 1.316(4) . ?
C9 N3 1.383(3) . ?
C9 C10 1.453(4) . ?
C10 C15 1.387(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.389(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.384(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.401(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.453(4) . ?
C16 N8 1.323(4) 3 ?
C16 N3 1.369(4) . ?
N1 Co1 1.924(2) . ?
N3 Co1 1.922(2) . ?
N8 C16 1.323(4) 3 ?
Co1 N3 1.922(2) 3 ?
Co1 N1 1.924(2) 3 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N8 C1 C2 C7 -179.7(3) . . . . ?
N1 C1 C2 C7 -0.2(3) . . . . ?
N8 C1 C2 C3 -1.5(5) . . . . ?
N1 C1 C2 C3 178.0(3) . . . . ?
C7 C2 C3 C4 -0.8(4) . . . . ?
C1 C2 C3 C4 -178.8(3) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C4 C5 C6 C7 1.1(5) . . . . ?
C5 C6 C7 C2 -1.0(4) . . . . ?
C5 C6 C7 C8 178.8(3) . . . . ?
C3 C2 C7 C6 0.9(4) . . . . ?
C1 C2 C7 C6 179.4(3) . . . . ?
C3 C2 C7 C8 -179.0(3) . . . . ?
C1 C2 C7 C8 -0.5(3) . . . . ?
C6 C7 C8 N2 1.6(5) . . . . ?
C2 C7 C8 N2 -178.6(2) . . . . ?
C6 C7 C8 N1 -178.7(3) . . . . ?
C2 C7 C8 N1 1.2(3) . . . . ?
N2 C9 C10 C15 -178.4(3) . . . . ?
N3 C9 C10 C15 1.1(3) . . . . ?
N2 C9 C10 C11 2.6(5) . . . . ?
N3 C9 C10 C11 -177.8(3) . . . . ?
C15 C10 C11 C12 0.0(4) . . . . ?
C9 C10 C11 C12 178.8(3) . . . . ?
C10 C11 C12 C13 0.0(5) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C13 C14 C15 -0.5(4) . . . . ?
C11 C10 C15 C14 -0.2(4) . . . . ?
C9 C10 C15 C14 -179.3(3) . . . . ?
C11 C10 C15 C16 179.0(3) . . . . ?
C9 C10 C15 C16 -0.2(3) . . . . ?
C13 C14 C15 C10 0.4(4) . . . . ?
C13 C14 C15 C16 -178.5(3) . . . . ?
C10 C15 C16 N8 -179.9(3) . . . 3 ?
C14 C15 C16 N8 -0.8(5) . . . 3 ?
C10 C15 C16 N3 -0.9(3) . . . . ?
C14 C15 C16 N3 178.2(3) . . . . ?
N8 C1 N1 C8 -179.6(3) . . . . ?
C2 C1 N1 C8 1.0(3) . . . . ?
N8 C1 N1 Co1 1.5(4) . . . . ?
C2 C1 N1 Co1 -177.96(18) . . . . ?
N2 C8 N1 C1 178.4(3) . . . . ?
C7 C8 N1 C1 -1.3(3) . . . . ?
N2 C8 N1 Co1 -2.7(4) . . . . ?
C7 C8 N1 Co1 177.60(18) . . . . ?
N3 C9 N2 C8 1.7(4) . . . . ?
C10 C9 N2 C8 -178.9(2) . . . . ?
N1 C8 N2 C9 1.1(4) . . . . ?
C7 C8 N2 C9 -179.3(3) . . . . ?
N8 C16 N3 C9 -179.5(3) 3 . . . ?
C15 C16 N3 C9 1.6(3) . . . . ?
N8 C16 N3 Co1 0.9(4) 3 . . . ?
C15 C16 N3 Co1 -178.03(18) . . . . ?
N2 C9 N3 C16 177.8(3) . . . . ?
C10 C9 N3 C16 -1.7(3) . . . . ?
N2 C9 N3 Co1 -2.6(4) . . . . ?
C10 C9 N3 Co1 177.93(18) . . . . ?
N1 C1 N8 C16 -3.0(5) . . . 3 ?
C2 C1 N8 C16 176.4(3) . . . 3 ?
