Controlling phase in low-nuclearity calixarene-capped porous coordination cages with ligand functionalization
Dworzak, Michael R.; Rowland, Casey A.; Yap, Glenn P. A.; Bloch, Eric D.; CrystEngComm  (2022) –; doi:10.1039/D2CE00861K

data_7245450
_publ_section_title
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 Controlling phase in low-nuclearity calixarene-capped porous coordination
 cages with ligand functionalization
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00861K
_journal_year                    2022
_chemical_formula_moiety         'C48 H64 Fe N2 O15 S4, 1[C3H7NO], 2[C2H6O]'
_chemical_formula_sum            'C55 H83 Fe N3 O18 S4'
_chemical_formula_weight         1258.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-17
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
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_audit_update_record
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2022-06-23 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.337(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.457(4)
_cell_length_b                   16.110(4)
_cell_length_c                   23.679(8)
_cell_measurement_reflns_used    52371
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      44.998
_cell_measurement_theta_min      2.714
_cell_volume                     6211(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0724
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52371
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        44.998
_diffrn_reflns_theta_max         44.998
_diffrn_reflns_theta_min         2.714
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.791
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.3980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1564 before and 0.1149 after correction.
The Ratio of minimum to maximum transmission is 0.5307.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.039(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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         4556
_refine_ls_number_restraints     680
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.1494
_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^)+(0.5000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4642
_refine_ls_wR_factor_ref         0.4707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4442
_reflns_number_total             4556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00861k2.cif
_cod_data_source_block           eric523
_cod_database_code               7245450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.429
_olex2_refinement_description
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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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(Fe1) = Uanis(Fe1A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(Fe1A)=1-FVAR(1)
 Sof(Fe1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C12(H12), C14(H14), C22(H22), C24(H24), C32(H32), C34(H34),
 C41(H41), C44(H44)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C48(H48A,H48B,H48C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
5.d Idealised tetrahedral OH refined as rotating group:
 O15(H15)
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_smtbx_masks_special_details
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A solvent mask was calculated and 388 electrons were 
found in a volume of 1508\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C3H7NO], 2[C2H6O] per Asymmetric Unit 
which account for 368 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27459
_shelx_hkl_checksum              88772
_shelx_fab_checksum              80331
_olex2_submission_special_instructions 'No special instructions were received'