Increasing the stability of calixarene-capped porous cages through coordination sphere tuning.
Dey, Avishek; Dworzak, Michael R.; Korathotage, Kaushalya D. P.; Ghosh, Munmun; Hoq, Jahidul; Montone, Christine M.; Yap, Glenn P. A.; Bloch, Eric D.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4005–4009; doi:10.1039/d3dt03365a

data_7714939
_publ_section_title
;
 Increasing the stability of calixarene-capped porous cages through
 coordination sphere tuning.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4005
_journal_page_last               4009
_journal_paper_doi               10.1039/d3dt03365a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C240 H228 Co16 N48 O52 S16, 2(C3 H7 N O), 28[C3H7NO], 6[CH3OH]'
_chemical_formula_sum            'C336 H462 Co16 N78 O88 S16'
_chemical_formula_weight         8457.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-06 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.673(4)
_cell_angle_beta                 97.371(4)
_cell_angle_gamma                98.450(5)
_cell_formula_units_Z            1
_cell_length_a                   12.3693(10)
_cell_length_b                   27.890(2)
_cell_length_c                   31.192(2)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.81
_cell_measurement_theta_min      2.52
_cell_volume                     10141.5(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Venture Photon'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79460
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        49.999
_diffrn_reflns_theta_max         49.999
_diffrn_reflns_theta_min         1.486
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.436
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1490 before and 0.1035 after correction.
The Ratio of minimum to maximum transmission is 0.6249.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1697
_refine_ls_number_reflns         20236
_refine_ls_number_restraints     2295
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.1014
_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/[\s^2^(Fo^2^)+(0.1677P)^2^+50.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2713
_refine_ls_wR_factor_ref         0.3079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12621
_reflns_number_total             20236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03365a2.cif
_cod_data_source_block           eric684
_cod_depositor_comments
'Adding full bibliography for 7714937--7714939.cif.'
_cod_original_cell_volume        10141.4(13)
_cod_database_code               7714939
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.271
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9_10-C9_10$1
 -2.7 with sigma of 0.002
 C7_10-C8_10 = C7_10-C9_10 = C7_10-C10_10
 1.534 with sigma of 0.011
 H1-O1
 0.98 with sigma of 0.02
 H2-O2
 0.98 with sigma of 0.02
 C7_10-C8_10 \\sim C7_10-C9_10 \\sim C7_10-C10_10
 with sigma of 0.02
 C8_10-C9_10 \\sim C9_10-C10_10 \\sim C10_10-C8_10
 with sigma of 0.02
 C7_10-C8A_10 \\sim C7_10-C9A_10 \\sim C7_10-C10A_10
 with sigma of 0.02
 C8A_10-C9A_10 \\sim C9A_10-C10A_10 \\sim C10A_10-C8A_10
 with sigma of 0.02
 C7_8-C8_8 \\sim C7_8-C9_8 \\sim C7_8-C10_8
 with sigma of 0.02
 C8_8-C9_8 \\sim C9_8-C10_8 \\sim C10_8-C8_8
 with sigma of 0.02
 O2-Co5 \\sim O2-Co6 \\sim O2-Co7 \\sim O2-Co8
 with sigma of 0.02
 H1-Co1 \\sim H1-Co2 \\sim H1-Co3 \\sim H1-Co4
 with sigma of 0.02
 H2-Co5 \\sim H2-Co6 \\sim H2-Co7 \\sim H2-Co8
 with sigma of 0.02
3. Restrained planarity
 C1_10, C2_10, C3_10, C4_10, C5_10, C6_10, C7_10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1_10 \\sim O2_10 \\sim O3_10 \\sim S1_10 \\sim C1_10 \\sim C2_10 \\sim C3_10
\\sim C4_10 \\sim C5_10 \\sim C6_10 \\sim C7_10 \\sim C8_10 \\sim C9_10 \\sim
C10_10: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
within 2A
O1_8 \\sim O2_8 \\sim O3_8 \\sim S1_8 \\sim C1_8 \\sim C2_8 \\sim C3_8 \\sim
C4_8 \\sim C5_8 \\sim C6_8 \\sim C7_8 \\sim C8_8 \\sim C9_8 \\sim C10_8: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
N1_6 \\sim N2_6 \\sim N3_6 \\sim N4_6 \\sim N5_6 \\sim N6_6 \\sim C1_6 \\sim
C2_6 \\sim C3_6 \\sim C4_6 \\sim C5_6 \\sim C6_6 \\sim C7_6 \\sim C8_6 \\sim
C9_6 \\sim C10_6: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Uanis(C9_10) = Uanis(C9A_10)
Uanis(C10_10) = Uanis(C10A_10)
Uanis(C8_10) = Uanis(C8A_10)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1_10, O2_10, O3_10, S1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10, C7_10,
 C8_10, C9_10, C10_10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1_8, O2_8, O3_8, S1_8, C1_8, C2_8, C3_8, C4_8, C5_8, C6_8, C7_8, C8_8, C9_8,
 C10_8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1_6, N2_6, N3_6, N4_6, N5_6, N6_6, C1_6, C2_6, C3_6, C4_6, C5_6, C6_6, C7_6,
 C8_6, C9_6, C10_6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
7.a Free rotating group:
 C4(C7,C8,C9,C10), C4(C7,C8,C9,C10)
7.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C8A(H8AA,H8AB,
 H8AC)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C3(H3), C5(H5), C3(H3), C5(H5), C3(H3), C5(H5), C1(H1),
 C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C1(H1), C3(H3), C5(H5), C6(H6),
 C7(H7), C10(H10), C3(H3), C5(H5), C3(H3), C5(H5), C3(H3), C5(H5), C1(H1),
 C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C1(H1), C3(H3), C5(H5), C6(H6),
 C7(H7), C10(H10), C1(H1), C3(H3), C5(H5)
7.d Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C3(C4,C5,C6,C7,C8)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1202 electrons were
found in a volume of 4570\%A^3^ in 3 voids per unit cell.
This is consistent with the presence of
28[C3H7NO], 6[CH3OH] per Asymmetric Unit
which account for 1228 electrons
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15287
_shelx_hkl_checksum              52211
_shelx_fab_checksum              1120
_olex2_submission_special_instructions 'No special instructions were received'