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_7714937
_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         'C336 H312 Fe24 N72 O78 S24, 88[C3H7NO]'
_chemical_formula_sum            'C600 H928 Fe24 N160 O166 S24'
_chemical_formula_weight         15148.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.4778(18)
_cell_length_b                   28.4778(18)
_cell_length_c                   47.720(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      50.54
_cell_measurement_theta_min      3.10
_cell_volume                     38700(4)
_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      120.00
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.1081
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            45037
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        51.187
_diffrn_reflns_theta_max         51.187
_diffrn_reflns_theta_min         1.806
_exptl_absorpt_coefficient_mu    4.775
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1217 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.6844.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       plate
_exptl_crystal_F_000             15968
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.000135(18)
_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   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10336
_refine_ls_number_restraints     599
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.1070
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3049
_refine_ls_wR_factor_ref         0.3359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5290
_reflns_number_total             10337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03365a2.cif
_cod_data_source_block           eric670
_cod_depositor_comments
'Adding full bibliography for 7714937--7714939.cif.'
_cod_original_cell_volume        38700(6)
_cod_database_code               7714937
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.527
_shelx_estimated_absorpt_t_min   0.309
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Free rotating group:
 C4(C7,C8,C9,C10), C4(C7,C8,C9,C10), C4(C7,C8,C9,C10)
3.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)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C1(H1), C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C3(H3),
 C5(H5), C3(H3), C5(H5)
3.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
3.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 7022 electrons were
found in a volume of 24551\%A^3^ in 1 void per unit cell.
This is consistent with the presence of
88[C3H7NO] per Asymmetric Unit
which account for 7040 electrons
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29766
_shelx_hkl_checksum              16224
_shelx_fab_checksum              40779
_olex2_submission_special_instructions 'No special instructions were received'