A ferromagnetically coupled pseudo-calixarene [Co16] wheel that self-assembles as a tubular network of capsules
Brechin, Euan K.; Tsami, Pinelopi A.; Tziotzi, Thomais G.; Tsanai, Angelos B.; Singh, Mukesh; Dalgarno, Scott; Milios, Constantinos J.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02554J

data_7711221
_publ_section_title
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 A ferromagnetically coupled pseudo-calixarene [Co16] wheel that
 self-assembles as a tubular network of capsules
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02554J
_journal_year                    2022
_chemical_formula_moiety         'C144 H128 Co16 O64, 8[CH3CN], 8[CH3CN]'
_chemical_formula_sum            'C176 H176 Co16 N16 O64'
_chemical_formula_weight         4482.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2022-06-09 deposited with the CCDC.	2022-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.9250(6)
_cell_length_b                   29.9250(6)
_cell_length_c                   11.2727(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      2.95
_cell_volume                     10094.8(4)
_computing_cell_refinement       'SAINT Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28843
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.261
_diffrn_reflns_theta_min         2.088
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.710
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1683 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.7396.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9197
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0436
_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/[\s^2^(Fo^2^)+(0.0774P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6880
_reflns_number_total             9197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02554j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        10094.8(5)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7711221
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.141
_shelx_estimated_absorpt_t_min   0.094
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29A-C28A = C28A-C27A = C27A-C26A = C26A-C25A = C26-C25 = C27-C26 = C28-C27 =
 C29-C28 = C30-C29 = C30-C25
 1.39 with sigma of 0.02
 C25A-C24 = C25-C24
 1.45 with sigma of 0.02
3. Restrained planarity
 C25A, C26A, C27A, C28A, C29A
 with sigma of 0.1
 C25, C26, C27, C28, C29
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C30) = Uanis(C25) = Uanis(C29) = Uanis(C26) = Uanis(C28) = Uanis(C27) =
Uanis(C25A) = Uanis(C29A) = Uanis(C26A) = Uanis(C28A) = Uanis(C27A)
5. Others
 Sof(H24A)=Sof(C25A)=Sof(C29A)=Sof(H29A)=Sof(C26A)=Sof(H26A)=Sof(C28A)=
 Sof(H28A)=Sof(C27A)=Sof(H27A)=1-FVAR(1)
 Sof(C25)=Sof(H24)=Sof(C29)=Sof(H29)=Sof(C26)=Sof(H26)=Sof(C28)=Sof(H28)=
 Sof(C27)=Sof(H27)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C2(H2), C22(H22), C23(H23), C15(H15), C16(H16), C10(H10),
 C3(H3), C24(H24), C24(H24A), C19(H19), C29(H29), C7(H7), C20(H20), C21(H21),
 C5(H5), C4(H4), C26(H26), C28(H28), C27(H27), C29A(H29A), C26A(H26A),
 C28A(H28A), C27A(H27A)
6.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C9(H9A,H9B,H9C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 756 electrons were 
found in a volume of 3428\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
8[CH3CN], 8[CH3CN] per Asymmetric Unit 
which account for 704 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93420
_shelx_hkl_checksum              73228
_shelx_fab_checksum              5829
_olex2_submission_special_instructions 'No special instructions were received'