#------------------------------------------------------------------------------
#$Date: 2022-01-29 05:01:03 +0200 (Sat, 29 Jan 2022) $
#$Revision: 272344 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/40/2244022.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2244022
loop_
_publ_author_name
'Park, Ava M.'
'Golen, James A.'
'Manke, David R.'
_publ_section_title
;
 A cuboidal [Cu₄(SO₄)₄] structure supported by β-picoline ligands
;
_journal_coeditor_code           ZL5027
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              108
_journal_page_last               110
_journal_paper_doi               10.1107/S2056989022000780
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Co4 (S O4)4 (C6 H7 N)8]'
_chemical_formula_moiety         'C48 H56 Co4 N8 O16 S4'
_chemical_formula_sum            'C48 H56 Co4 N8 O16 S4'
_chemical_formula_weight         1364.96
_chemical_name_systematic
;
Tetra-μ₃-sulfato-tetrakis[bis(3-methylpyridine)cobalt(II)]
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6121(16)
_cell_length_b                   15.6121(16)
_cell_length_c                   11.8359(13)
_cell_measurement_reflns_used    9496
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.92
_cell_volume                     2884.9(5)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54595
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         2.917
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2018)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.201
_refine_ls_abs_structure_details
;
Flack x determined using 1117 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       0.0049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0190
_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)+(0.0165P)²+1.2064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                2624
_reflns_number_total             2744
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zl5027sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2884.9(7)
_cod_database_code               2244022
_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   0.738
_shelx_estimated_absorpt_t_max   0.774
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.64636(2) 0.49053(2) 0.41389(3) 0.02066(11) Uani d 1 . .
S S1 0.52522(4) 0.64004(4) 0.35520(5) 0.02043(15) Uani d 1 . .
O O1 0.58168(12) 0.57205(12) 0.30908(15) 0.0267(4) Uani d 1 . .
O O2 0.49144(15) 0.69145(13) 0.26473(17) 0.0370(5) Uani d 1 . .
O O3 0.45605(11) 0.59894(11) 0.42553(16) 0.0240(4) Uani d 1 . .
O O4 0.57304(12) 0.69234(11) 0.43961(15) 0.0258(4) Uani d 1 . .
N N1 0.75982(14) 0.57112(15) 0.4121(2) 0.0319(5) Uani d 1 . .
N N2 0.70169(16) 0.42286(15) 0.2775(2) 0.0293(5) Uani d 1 . .
C C1 0.82170(19) 0.5691(2) 0.4896(3) 0.0400(7) Uani d 1 . .
H H1 0.813680 0.534627 0.552786 0.048 Uiso calc 1 . .
C C2 0.8976(2) 0.6156(2) 0.4819(3) 0.0489(8) Uani d 1 . .
C C3 0.9084(2) 0.6660(2) 0.3863(3) 0.0546(10) Uani d 1 . .
H H3 0.958296 0.697697 0.376688 0.065 Uiso calc 1 . .
C C4 0.8451(2) 0.6690(2) 0.3064(3) 0.0541(10) Uani d 1 . .
H H4 0.851466 0.702977 0.242445 0.065 Uiso calc 1 . .
C C5 0.7719(2) 0.6210(2) 0.3218(3) 0.0434(8) Uani d 1 . .
H H5 0.729157 0.623471 0.267110 0.052 Uiso calc 1 . .
C C6 0.9650(3) 0.6110(3) 0.5724(4) 0.0829(15) Uani d 1 . .
H H6A 0.946445 0.572676 0.630913 0.124 Uiso calc 1 . .
H H6B 0.973938 0.667009 0.603611 0.124 Uiso calc 1 . .
H H6C 1.017567 0.590328 0.540358 0.124 Uiso calc 1 . .
C C7 0.6638(2) 0.4183(2) 0.1768(3) 0.0340(7) Uani d 1 . .
H H7 0.611734 0.446338 0.167140 0.041 Uiso calc 1 . .
C C8 0.6978(2) 0.3738(2) 0.0853(3) 0.0422(7) Uani d 1 . .
C C9 0.7741(2) 0.3311(2) 0.1032(3) 0.0499(9) Uani d 1 . .
H H9 0.798504 0.299413 0.045000 0.060 Uiso calc 1 . .
C C10 0.8143(2) 0.3351(2) 0.2062(3) 0.0490(9) Uani d 1 . .
H H10 0.865907 0.306837 0.218114 0.059 Uiso calc 1 . .
C C11 0.7766(2) 0.3817(2) 0.2914(3) 0.0386(8) Uani d 1 . .
H H11 0.803962 0.384829 0.361126 0.046 Uiso calc 1 . .
C C12 0.6512(3) 0.3707(3) -0.0255(3) 0.0732(12) Uani d 1 . .
H H12A 0.590895 0.377919 -0.012705 0.110 Uiso calc 1 . .
H H12B 0.661205 0.316328 -0.061099 0.110 Uiso calc 1 . .
H H12C 0.671634 0.415746 -0.073630 0.110 Uiso calc 1 . .
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'
Co Co 0.3494 0.9721 '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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Co1 S1 . 3_566 129.94(5) ?
O1 Co1 O3 . 2_665 94.41(7) ?
O1 Co1 O3 . 3_566 97.00(7) ?
O1 Co1 O4 . 3_566 162.52(7) ?
O1 Co1 N1 . . 92.08(9) ?
O1 Co1 N2 . . 92.84(9) ?
O3 Co1 S1 3_566 3_566 33.21(5) ?
O3 Co1 S1 2_665 3_566 81.36(5) ?
O3 Co1 O3 2_665 3_566 86.57(8) ?
O3 Co1 N1 2_665 . 173.44(9) ?
O4 Co1 S1 3_566 3_566 32.58(5) ?
O4 Co1 O3 3_566 2_665 83.94(7) ?
O4 Co1 O3 3_566 3_566 65.55(7) ?
O4 Co1 N1 3_566 . 90.16(9) ?
N1 Co1 S1 . 3_566 95.20(8) ?
N1 Co1 O3 . 3_566 93.61(8) ?
N2 Co1 S1 . 3_566 136.90(7) ?
N2 Co1 O3 . 3_566 170.11(9) ?
N2 Co1 O3 . 2_665 91.63(8) ?
N2 Co1 O4 . 3_566 104.59(8) ?
N2 Co1 N1 . . 87.07(9) ?
O1 S1 Co1 . 4_656 116.43(7) ?
O1 S1 O3 . . 108.92(10) ?
O1 S1 O4 . . 109.93(11) ?
O2 S1 Co1 . 4_656 133.48(9) ?
O2 S1 O1 . . 110.07(11) ?
O2 S1 O3 . . 112.71(12) ?
O2 S1 O4 . . 112.15(12) ?
O3 S1 Co1 . 4_656 53.22(7) ?
O4 S1 Co1 . 4_656 50.06(7) ?
O4 S1 O3 . . 102.82(11) ?
S1 O1 Co1 . . 121.04(10) ?
Co1 O3 Co1 2_665 4_656 124.11(9) ?
S1 O3 Co1 . 2_665 141.48(12) ?
S1 O3 Co1 . 4_656 93.57(9) ?
S1 O4 Co1 . 4_656 97.36(9) ?
C1 N1 Co1 . . 124.8(2) ?
C1 N1 C5 . . 117.5(3) ?
C5 N1 Co1 . . 117.4(2) ?
C7 N2 Co1 . . 121.9(2) ?
C7 N2 C11 . . 118.1(3) ?
C11 N2 Co1 . . 120.0(2) ?
N1 C1 H1 . . 118.0 ?
N1 C1 C2 . . 124.0(3) ?
C2 C1 H1 . . 118.0 ?
C1 C2 C6 . . 121.6(4) ?
C3 C2 C1 . . 116.9(3) ?
C3 C2 C6 . . 121.5(3) ?
C2 C3 H3 . . 120.2 ?
C4 C3 C2 . . 119.7(3) ?
C4 C3 H3 . . 120.2 ?
C3 C4 H4 . . 120.4 ?
C3 C4 C5 . . 119.3(3) ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 122.6(4) ?
N1 C5 H5 . . 118.7 ?
C4 C5 H5 . . 118.7 ?
C2 C6 H6A . . 109.5 ?
C2 C6 H6B . . 109.5 ?
C2 C6 H6C . . 109.5 ?
H6A C6 H6B . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N2 C7 H7 . . 118.2 ?
N2 C7 C8 . . 123.6(3) ?
C8 C7 H7 . . 118.2 ?
C7 C8 C12 . . 120.8(3) ?
C9 C8 C7 . . 116.8(3) ?
C9 C8 C12 . . 122.4(3) ?
C8 C9 H9 . . 119.7 ?
C10 C9 C8 . . 120.6(3) ?
C10 C9 H9 . . 119.7 ?
C9 C10 H10 . . 120.6 ?
C9 C10 C11 . . 118.7(3) ?
C11 C10 H10 . . 120.6 ?
N2 C11 C10 . . 122.3(3) ?
N2 C11 H11 . . 118.9 ?
C10 C11 H11 . . 118.9 ?
C8 C12 H12A . . 109.5 ?
C8 C12 H12B . . 109.5 ?
C8 C12 H12C . . 109.5 ?
H12A C12 H12B . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 S1 3_566 2.7458(7) ?
Co1 O1 . 2.0441(19) ?
Co1 O3 3_566 2.2037(19) ?
Co1 O3 2_665 2.1274(18) ?
Co1 O4 3_566 2.1229(18) ?
Co1 N1 . 2.173(2) ?
Co1 N2 . 2.114(2) ?
S1 O1 . 1.4839(19) ?
S1 O2 . 1.438(2) ?
S1 O3 . 1.5069(18) ?
S1 O4 . 1.491(2) ?
N1 C1 . 1.332(4) ?
N1 C5 . 1.336(4) ?
N2 C7 . 1.333(4) ?
N2 C11 . 1.345(4) ?
C1 H1 . 0.9300 ?
C1 C2 . 1.392(4) ?
C2 C3 . 1.389(5) ?
C2 C6 . 1.503(5) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.368(6) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.379(5) ?
C5 H5 . 0.9300 ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C7 H7 . 0.9300 ?
C7 C8 . 1.391(4) ?
C8 C9 . 1.382(5) ?
C8 C12 . 1.501(5) ?
C9 H9 . 0.9300 ?
C9 C10 . 1.371(6) ?
C10 H10 . 0.9300 ?
C10 C11 . 1.376(5) ?
C11 H11 . 0.9300 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1 H1 O4 3_566 0.93 2.53 3.116(4) 120.9 yes
C3 H3 O2 6_565 0.93 2.46 3.135(4) 129.3 yes
C5 H5 O1 . 0.93 2.49 3.070(4) 120.7 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Co1 S1 O1 Co1 4_656 . . . -1.75(15) ?
Co1 S1 O3 Co1 4_656 . . 2_665 -168.6(2) ?
Co1 N1 C1 C2 . . . . 173.9(3) ?
Co1 N1 C5 C4 . . . . -174.0(3) ?
Co1 N2 C7 C8 . . . . -179.4(2) ?
Co1 N2 C11 C10 . . . . 178.4(2) ?
O1 S1 O3 Co1 . . . 4_656 109.34(9) ?
O1 S1 O3 Co1 . . . 2_665 -59.3(2) ?
O1 S1 O4 Co1 . . . 4_656 -108.29(10) ?
O2 S1 O1 Co1 . . . . 176.64(13) ?
O2 S1 O3 Co1 . . . 4_656 -128.20(11) ?
O2 S1 O3 Co1 . . . 2_665 63.1(2) ?
O2 S1 O4 Co1 . . . 4_656 128.92(11) ?
O3 S1 O1 Co1 . . . . -59.31(15) ?
O3 S1 O4 Co1 . . . 4_656 7.57(11) ?
O4 S1 O1 Co1 . . . . 52.63(15) ?
O4 S1 O3 Co1 . . . 2_665 -175.90(17) ?
O4 S1 O3 Co1 . . . 4_656 -7.25(10) ?
N1 C1 C2 C3 . . . . -0.5(5) ?
N1 C1 C2 C6 . . . . 179.7(4) ?
N2 C7 C8 C9 . . . . 1.5(5) ?
N2 C7 C8 C12 . . . . 179.5(3) ?
C1 N1 C5 C4 . . . . 0.4(5) ?
C1 C2 C3 C4 . . . . 0.8(5) ?
C2 C3 C4 C5 . . . . -0.6(6) ?
C3 C4 C5 N1 . . . . -0.1(6) ?
C5 N1 C1 C2 . . . . -0.1(5) ?
C6 C2 C3 C4 . . . . -179.4(4) ?
C7 N2 C11 C10 . . . . -0.6(4) ?
C7 C8 C9 C10 . . . . -1.5(5) ?
C8 C9 C10 C11 . . . . 0.6(5) ?
C9 C10 C11 N2 . . . . 0.5(5) ?
C11 N2 C7 C8 . . . . -0.5(4) ?
C12 C8 C9 C10 . . . . -179.4(3) ?

_cod_database_fobs_code 2244022
