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#$Revision: 300684 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/03/7250377.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_7250377
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 H76 Co7 N8 O29'
_chemical_formula_weight         1773.81
_chemical_name_common            '[2-Fur-Co7].3H2O'
_chemical_name_systematic        2-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                   14.100(2)
_cell_length_b                   14.100(2)
_cell_length_c                   22.702(5)
_cell_measurement_reflns_used    3532
_cell_measurement_temperature    149.9(1)
_cell_measurement_theta_max      29.1934
_cell_measurement_theta_min      2.8834
_cell_volume                     3908.7(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      149.9(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  0.0409
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            2388
_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         25.349
_diffrn_reflns_theta_min         2.889
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68343
_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
_platon_squeeze_details
;
;
_refine_diff_density_max         2.231
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_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      1.071
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0777
_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)+(0.1187P)²+24.3244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1894
_reflns_number_total             2388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00341e2.cif
_cod_data_source_block           sm200sq
_cod_depositor_comments
'Adding full bibliography for 7250376--7250384.cif.'
_cod_original_cell_volume        3908.7(14)
_cod_database_code               7250377
_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   0.895
_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 0.0255(5) Uani 1 6 d S T P . .
O1 O -0.0048(4) -0.1312(3) 0.0460(2) 0.0320(10) Uani 1 1 d . . . . .
H1 H 0.007528 -0.125803 0.089580 0.038 Uiso 1 1 calc R U . . .
N1 N -0.1934(5) -0.3772(5) 0.0763(3) 0.0427(15) Uani 1 1 d . . . . .
C1 C -0.1277(8) -0.4316(8) 0.0796(4) 0.062(3) Uani 1 1 d . . . . .
H1A H -0.158339 -0.488987 0.109773 0.093 Uiso 1 1 calc R U . . .
H1B H -0.051983 -0.377691 0.089935 0.093 Uiso 1 1 calc R U . . .
H1C H -0.128914 -0.464375 0.041355 0.093 Uiso 1 1 calc R U . . .
Co2 Co -0.14484(7) -0.25498(7) 0.01217(4) 0.0324(4) Uani 1 1 d . . . . .
O2 O -0.2762(3) -0.2441(4) 0.03378(19) 0.0307(10) Uani 1 1 d . . . . .
N2 N -0.666667 -0.333333 0.2938(6) 0.054(3) Uani 1 3 d S T P . .
C2 C -0.2719(6) -0.4096(6) 0.1122(3) 0.0446(18) Uani 1 1 d . . . . .
H2 H -0.284961 -0.468312 0.137715 0.053 Uiso 1 1 calc R U . . .
O3 O -0.4002(4) -0.1612(4) 0.0530(2) 0.0399(12) Uani 1 1 d . . . . .
C3 C -0.3447(6) -0.3636(6) 0.1175(3) 0.0359(15) Uani 1 1 d . . . . .
O4 O -0.6562(8) -0.4146(8) 0.2909(4) 0.104(3) Uani 1 1 d . . . . .
C4 C -0.4212(6) -0.4036(7) 0.1662(3) 0.0421(17) Uani 1 1 d . . . . .
H4 H -0.426161 -0.459823 0.191219 0.051 Uiso 1 1 calc R U . . .
C5 C -0.4860(6) -0.3587(7) 0.1752(3) 0.0476(19) Uani 1 1 d . . . . .
H5 H -0.534817 -0.383534 0.207733 0.057 Uiso 1 1 calc R U . . .
C6 C -0.4840(6) -0.2787(7) 0.1392(3) 0.0428(17) Uani 1 1 d . . . . .
H6 H -0.530451 -0.249284 0.146614 0.051 Uiso 1 1 calc R U . . .
C7 C -0.4127(5) -0.2430(6) 0.0922(3) 0.0349(16) Uani 1 1 d . . . . .
C8 C -0.3414(5) -0.2842(5) 0.0802(3) 0.0271(13) Uani 1 1 d . . . . .
C9 C -0.4935(6) -0.1474(6) 0.0437(4) 0.051(2) Uani 1 1 d . . . . .
H9A H -0.559197 -0.219223 0.038529 0.077 Uiso 1 1 calc R U . . .
H9B H -0.481731 -0.102846 0.008405 0.077 Uiso 1 1 calc R U . . .
H9C H -0.503027 -0.110581 0.077939 0.077 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'
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 180.0 7 . ?
O1 Co1 O1 97.30(16) 7 8 ?
O1 Co1 O1 82.70(16) . 8 ?
O1 Co1 O1 82.70(16) 7 2 ?
O1 Co1 O1 97.30(16) . 2 ?
O1 Co1 O1 180.0(5) 8 2 ?
O1 Co1 O1 97.29(16) 7 9 ?
O1 Co1 O1 82.71(16) . 9 ?
O1 Co1 O1 97.29(16) 8 9 ?
O1 Co1 O1 82.71(16) 2 9 ?
O1 Co1 O1 82.71(16) 7 3 ?
O1 Co1 O1 97.29(16) . 3 ?
O1 Co1 O1 82.71(16) 8 3 ?
O1 Co1 O1 97.29(16) 2 3 ?
O1 Co1 O1 180.0(3) 9 3 ?
Co2 O1 Co1 99.15(19) . . ?
Co2 O1 Co2 98.15(18) . 9 ?
Co1 O1 Co2 94.52(18) . 9 ?
Co2 O1 H1 119.9 . . ?
Co1 O1 H1 119.9 . . ?
Co2 O1 H1 119.9 9 . ?
C2 N1 C1 116.5(6) . . ?
C2 N1 Co2 127.8(5) . . ?
C1 N1 Co2 115.7(5) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Co2 O1 112.55(18) . . ?
O2 Co2 O2 163.05(10) . 9 ?
O1 Co2 O2 79.93(17) . 9 ?
O2 Co2 N1 87.6(2) . . ?
O1 Co2 N1 102.9(2) . . ?
O2 Co2 N1 101.1(2) 9 . ?
O2 Co2 O1 77.52(17) . 8 ?
O1 Co2 O1 82.5(2) . 8 ?
O2 Co2 O1 93.48(18) 9 8 ?
N1 Co2 O1 165.1(2) . 8 ?
O2 Co2 O3 94.63(18) . 9 ?
O1 Co2 O3 151.84(17) . 9 ?
O2 Co2 O3 71.97(17) 9 9 ?
N1 Co2 O3 84.8(2) . 9 ?
O1 Co2 O3 96.98(18) 8 9 ?
C8 O2 Co2 129.5(4) . . ?
C8 O2 Co2 123.4(4) . 8 ?
Co2 O2 Co2 103.47(19) . 8 ?
O4 N2 O4 119.73(16) 3_445 2_455 ?
O4 N2 O4 119.73(16) 3_445 . ?
O4 N2 O4 119.73(16) 2_455 . ?
N1 C2 C3 125.1(7) . . ?
N1 C2 H2 117.5 . . ?
C3 C2 H2 117.5 . . ?
C7 O3 C9 117.3(6) . . ?
C7 O3 Co2 112.8(4) . 8 ?
C9 O3 Co2 126.0(5) . 8 ?
C8 C3 C4 120.0(6) . . ?
C8 C3 C2 123.8(6) . . ?
C4 C3 C2 116.1(6) . . ?
C5 C4 C3 118.4(7) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 123.1(7) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C7 C6 C5 118.0(7) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 O3 124.3(7) . . ?
C6 C7 C8 122.5(7) . . ?
O3 C7 C8 113.2(6) . . ?
O2 C8 C3 124.6(6) . . ?
O2 C8 C7 117.5(6) . . ?
C3 C8 C7 117.9(6) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 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 2.096(4) 7 ?
Co1 O1 2.096(4) . ?
Co1 O1 2.096(4) 8 ?
Co1 O1 2.096(4) 2 ?
Co1 O1 2.096(4) 9 ?
Co1 O1 2.096(4) 3 ?
O1 Co2 2.023(4) . ?
O1 Co2 2.173(4) 9 ?
O1 H1 1.0000 . ?
N1 C2 1.262(9) . ?
N1 C1 1.471(10) . ?
N1 Co2 2.093(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Co2 O2 1.995(4) . ?
Co2 O2 2.045(4) 9 ?
Co2 O3 2.329(5) 9 ?
O2 C8 1.324(7) . ?
N2 O4 1.229(9) 3_445 ?
N2 O4 1.229(9) 2_455 ?
N2 O4 1.229(9) . ?
C2 C3 1.468(10) . ?
C2 H2 0.9500 . ?
O3 C7 1.397(9) . ?
O3 C9 1.438(8) . ?
C3 C8 1.386(9) . ?
C3 C4 1.446(10) . ?
C4 C5 1.362(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.417(9) . ?
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 0.250 477 83 ' '
2 0.000 0.000 0.750 477 83 ' '
3 0.333 0.667 0.429 16 3 ' '
4 0.333 0.666 0.929 16 3 ' '
5 0.666 0.333 0.071 16 3 ' '
6 0.666 0.333 0.571 16 3 ' '
