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#$Revision: 300684 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/03/7250380.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_7250380
loop_
_publ_author_name
'Slater-Parry, Mari'
'Meally, Seán T.'
'Ratanasakprakan, Chotima'
'Townrow, David E.'
'Ellaby, Rebecca J.'
'Page, Samuel J.'
'Jones, Leigh F.'
_publ_section_title
;
 Pseudo [M(ii)7] (M = Co, Ni and Zn) metallocalix[6]arene hosts
 encapsulate a range of organic guest molecules in the solid state
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3823
_journal_page_last               3832
_journal_paper_doi               10.1039/D5CE00341E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C59 H79 Co7 N8 O30.5'
_chemical_formula_weight         1800.83
_chemical_name_common            '[3-fur-Co7].4.5H2O'
_chemical_name_systematic        3-Fur-Co7
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.098(2)
_cell_length_b                   14.098(2)
_cell_length_c                   22.706(5)
_cell_measurement_reflns_used    2502
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      29.0946
_cell_measurement_theta_min      3.0197
_cell_volume                     3908.3(12)
_computing_cell_refinement
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_collection
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_reduction
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_molecular_graphics
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7890
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.026
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1654
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0936
_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)+(0.1391P)²+11.4781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2519
_refine_ls_wR_factor_ref         0.2778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1561
_reflns_number_total             2388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00341e2.cif
_cod_data_source_block           sm353asq
_cod_depositor_comments
'Adding full bibliography for 7250376--7250384.cif.'
_cod_original_cell_volume        3908.5(14)
_cod_database_code               7250380
_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   0.888
_shelx_estimated_absorpt_t_max   0.942
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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
Co1 Co 0.000000 0.000000 0.000000 0.0309(7) Uani 1 6 d S T P . .
O1 O -0.1265(4) 0.0042(4) -0.0465(2) 0.0369(14) Uani 1 1 d . . . . .
H1 H -0.133565 -0.008090 -0.089987 0.044 Uiso 1 1 calc R U . . .
N1 N -0.1837(6) 0.1942(7) -0.0759(3) 0.0464(19) Uani 1 1 d . . . . .
C1 C 0.3460(8) 0.4912(8) -0.0453(5) 0.060(3) Uani 1 1 d . . . . .
H1A H 0.393256 0.494011 -0.077747 0.090 Uiso 1 1 calc R U . . .
H1B H 0.376198 0.483818 -0.007874 0.090 Uiso 1 1 calc R U . . .
H1C H 0.342221 0.558748 -0.044974 0.090 Uiso 1 1 calc R U . . .
Co2 Co -0.11025(10) 0.14407(10) -0.01214(5) 0.0385(5) Uani 1 1 d . . . . .
O2 O 0.0320(4) 0.2752(5) -0.0346(2) 0.0362(13) Uani 1 1 d . . . . .
N2 N 0.333333 0.666667 -0.2927(7) 0.057(4) Uani 1 3 d S T P . .
C2 C 0.1690(7) 0.4117(7) -0.0921(4) 0.039(2) Uani 1 1 d . . . . .
O3 O 0.2379(5) 0.3988(5) -0.0533(3) 0.0466(16) Uani 1 1 d . . . . .
C3 C 0.2049(9) 0.4844(9) -0.1382(4) 0.055(3) Uani 1 1 d . . . . .
H3 H 0.280942 0.532457 -0.144607 0.066 Uiso 1 1 calc R U . . .
O4 O 0.2404(8) 0.6537(8) -0.2917(4) 0.099(3) Uani 1 1 d . . . . .
C4 C 0.1257(9) 0.4857(8) -0.1758(4) 0.054(3) Uani 1 1 d . . . . .
H4 H 0.149308 0.533783 -0.208743 0.065 Uiso 1 1 calc R U . . .
C5 C 0.0181(8) 0.4209(8) -0.1663(4) 0.044(2) Uani 1 1 d . . . . .
H5 H -0.033205 0.425558 -0.191503 0.053 Uiso 1 1 calc R U . . .
C6 C -0.0204(8) 0.3441(7) -0.1180(4) 0.046(2) Uani 1 1 d . . . . .
C7 C 0.0564(7) 0.3415(6) -0.0798(3) 0.0298(17) Uani 1 1 d . . . . .
C8 C -0.1390(8) 0.2721(8) -0.1119(4) 0.046(2) Uani 1 1 d . . . . .
H8 H -0.185280 0.285091 -0.136950 0.055 Uiso 1 1 calc R U . . .
C9 C -0.3075(8) 0.1251(10) -0.0799(5) 0.070(3) Uani 1 1 d . . . . .
H9A H -0.334812 0.158806 -0.107857 0.106 Uiso 1 1 calc R U . . .
H9B H -0.339636 0.120495 -0.041045 0.106 Uiso 1 1 calc R U . . .
H9C H -0.327853 0.051307 -0.093525 0.106 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'
N N 0.0061 0.0033 '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'
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'
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
O1 Co1 O1 83.0(2) . 8 ?
O1 Co1 O1 97.0(2) . 2 ?
O1 Co1 O1 180.0(4) 8 2 ?
O1 Co1 O1 180.0 . 7 ?
O1 Co1 O1 97.0(2) 8 7 ?
O1 Co1 O1 83.0(2) 2 7 ?
O1 Co1 O1 83.0(2) . 9 ?
O1 Co1 O1 97.0(2) 8 9 ?
O1 Co1 O1 83.0(2) 2 9 ?
O1 Co1 O1 97.0(2) 7 9 ?
O1 Co1 O1 97.0(2) . 3 ?
O1 Co1 O1 83.0(2) 8 3 ?
O1 Co1 O1 97.0(2) 2 3 ?
O1 Co1 O1 83.0(2) 7 3 ?
O1 Co1 O1 180.0(6) 9 3 ?
Co2 O1 Co1 98.6(2) . . ?
Co2 O1 Co2 97.8(2) . 9 ?
Co1 O1 Co2 94.1(2) . 9 ?
Co2 O1 H1 120.2 . . ?
Co1 O1 H1 120.2 . . ?
Co2 O1 H1 120.2 9 . ?
C8 N1 C9 115.7(8) . . ?
C8 N1 Co2 128.9(7) . . ?
C9 N1 Co2 115.4(6) . . ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Co2 O1 112.1(2) . . ?
O2 Co2 O2 163.02(13) . 9 ?
O1 Co2 O2 80.4(2) . 9 ?
O2 Co2 N1 87.1(3) . . ?
O1 Co2 N1 103.2(3) . . ?
O2 Co2 N1 101.7(3) 9 . ?
O2 Co2 O1 77.9(2) . 8 ?
O1 Co2 O1 83.1(3) . 8 ?
O2 Co2 O1 92.8(2) 9 8 ?
N1 Co2 O1 164.9(3) . 8 ?
O2 Co2 O3 95.1(2) . 9 ?
O1 Co2 O3 151.9(2) . 9 ?
O2 Co2 O3 71.6(2) 9 9 ?
N1 Co2 O3 84.6(3) . 9 ?
O1 Co2 O3 96.3(2) 8 9 ?
C7 O2 Co2 130.0(5) . . ?
C7 O2 Co2 124.2(5) . 8 ?
Co2 O2 Co2 103.0(2) . 8 ?
O4 N2 O4 119.97(7) . 3_565 ?
O4 N2 O4 119.97(7) . 2_665 ?
O4 N2 O4 119.97(7) 3_565 2_665 ?
C3 C2 O3 124.1(8) . . ?
C3 C2 C7 122.6(9) . . ?
O3 C2 C7 113.4(7) . . ?
C2 O3 C1 117.1(7) . . ?
C2 O3 Co2 113.0(5) . 8 ?
C1 O3 Co2 126.4(6) . 8 ?
C2 C3 C4 118.2(10) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 121.7(9) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 120.5(9) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.0(9) . . ?
C7 C6 C8 123.5(9) . . ?
C5 C6 C8 117.5(8) . . ?
O2 C7 C6 124.9(8) . . ?
O2 C7 C2 117.0(7) . . ?
C6 C7 C2 118.1(8) . . ?
N1 C8 C6 124.5(9) . . ?
N1 C8 H8 117.8 . . ?
C6 C8 H8 117.8 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
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
Co1 O1 2.099(5) . ?
Co1 O1 2.099(5) 8 ?
Co1 O1 2.099(5) 2 ?
Co1 O1 2.099(5) 7 ?
Co1 O1 2.099(5) 9 ?
Co1 O1 2.099(5) 3 ?
O1 Co2 2.023(6) . ?
O1 Co2 2.171(6) 9 ?
O1 H1 1.0000 . ?
N1 C8 1.258(11) . ?
N1 C9 1.518(12) . ?
N1 Co2 2.096(7) . ?
C1 O3 1.438(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Co2 O2 1.998(5) . ?
Co2 O2 2.043(6) 9 ?
Co2 O3 2.327(6) 9 ?
O2 C7 1.314(9) . ?
N2 O4 1.229(10) . ?
N2 O4 1.229(10) 3_565 ?
N2 O4 1.229(10) 2_665 ?
C2 C3 1.372(13) . ?
C2 O3 1.388(11) . ?
C2 C7 1.417(12) . ?
C3 C4 1.415(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.340(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.442(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.402(12) . ?
C6 C8 1.466(13) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 479 98 ' '
2 0.000 0.000 0.750 479 98 ' '
3 0.333 0.667 0.561 21 4 ' '
4 0.333 0.667 0.061 21 4 ' '
5 0.667 0.333 0.939 21 4 ' '
6 0.667 0.333 0.439 21 4 ' '
