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_7245448
_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         'C210 H170 Co8 N4 O42 S8, 14[C3H7NO]'
_chemical_formula_sum            'C210 H170 Co8 N4 O42 S8'
_chemical_formula_weight         4149.41
_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             2021-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 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                 101.993(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.571(3)
_cell_length_b                   22.245(3)
_cell_length_c                   23.653(3)
_cell_measurement_reflns_used    9026
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      40.08
_cell_measurement_theta_min      2.97
_cell_volume                     12131(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60088
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        40.144
_diffrn_reflns_theta_max         40.144
_diffrn_reflns_theta_min         1.916
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.332
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1420 before and 0.1046 after correction.
The Ratio of minimum to maximum transmission is 0.6640.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             4276
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         7155
_refine_ls_number_restraints     2560
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.1129
_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^)+(0.0545P)^2^+276.8382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5983
_reflns_number_total             7155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00861k2.cif
_cod_data_source_block           eric496
_cod_database_code               7245448
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.392
_olex2_refinement_description
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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
 C33-C36
 1.504 with sigma of 0.014
 C71-C72B \\sim C71-C73B \\sim C71-C74B
 with sigma of 0.02
 C68-C72B \\sim C68-C73B \\sim C68-C74B
 with sigma of 0.02
 C72B-C73B \\sim C73B-C74B \\sim C74B-C72B
 with sigma of 0.02
 C81-C82B \\sim C81-C83B \\sim C81-C84B
 with sigma of 0.02
 C82B-C83B \\sim C83B-C84B \\sim C84B-C82B
 with sigma of 0.02
 C101-C102 \\sim C101-C103 \\sim C101-C104
 with sigma of 0.02
 C102-C103 \\sim C103-C104 \\sim C104-C102
 with sigma of 0.02
 C91-C92A \\sim C91-C93A \\sim C91-C93A \\sim C91-C92B \\sim C91-C93B \\sim
C91-C93B
 with sigma of 0.02
 C92A-C93A \\sim C93A-C94A \\sim C94A-C92A \\sim C92B-C93B \\sim C93B-C94B
\\sim C94B-C92B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C71) \\sim Ueq, Uanis(C72A) \\sim Ueq, Uanis(C73A) \\sim Ueq, Uanis(C74A)
\\sim Ueq, Uanis(C72B) \\sim Ueq, Uanis(C73B) \\sim Ueq, Uanis(C74B) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74A) = Uanis(C74B)
Uanis(C72A) = Uanis(C72B)
Uanis(C73A) = Uanis(C73B)
Uanis(C82A) = Uanis(C82B)
Uanis(C83A) = Uanis(C83B)
Uanis(C84A) = Uanis(C84B)
Uanis(C92A) = Uanis(C92B)
Uanis(C93A) = Uanis(C93B)
Uanis(C94A) = Uanis(C94B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C92B)=Sof(H92D)=Sof(H92E)=Sof(H92F)=Sof(C93B)=Sof(H93D)=Sof(H93E)=
 Sof(H93F)=Sof(C94B)=Sof(H94D)=Sof(H94E)=Sof(H94F)=1-FVAR(1)
 Sof(C92A)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(C93A)=Sof(H93A)=Sof(H93B)=
 Sof(H93C)=Sof(C94A)=Sof(H94A)=Sof(H94B)=Sof(H94C)=FVAR(1)
 Sof(C82B)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C83B)=Sof(H83D)=Sof(H83E)=
 Sof(H83F)=Sof(C84B)=Sof(H84D)=Sof(H84E)=Sof(H84F)=1-FVAR(2)
 Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83A)=Sof(H83A)=Sof(H83B)=
 Sof(H83C)=Sof(C84A)=Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(2)
 Sof(C72B)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C73B)=Sof(H73D)=Sof(H73E)=
 Sof(H73F)=Sof(C74B)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(3)
 Sof(C72A)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C73A)=Sof(H73A)=Sof(H73B)=
 Sof(H73C)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(3)
6.a Me refined with riding coordinates:
 C1O(H1OA,H1OB,H1OC), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,
 H10H,H10I), C72A(H72A,H72B,H72C), C73A(H73A,H73B,H73C), C74A(H74A,H74B,H74C),
 C82A(H82A,H82B,H82C), C83A(H83A,H83B,H83C), C84A(H84A,H84B,H84C), C92A(H92A,
 H92B,H92C), C93A(H93A,H93B,H93C), C94A(H94A,H94B,H94C), C72B(H72D,H72E,H72F),
 C73B(H73D,H73E,H73F), C74B(H74D,H74E,H74F), C82B(H82D,H82E,H82F), C83B(H83D,
 H83E,H83F), C84B(H84D,H84E,H84F), C92B(H92D,H92E,H92F), C93B(H93D,H93E,H93F),
 C94B(H94D,H94E,H94F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C35(H35), C38(H38), C41(H41), C44(H44),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C67(H67), C69(H69), C77(H77), C79(H79), C87(H87), C89(H89), C97(H97), C99(H99)
6.c Fitted hexagon refined as free rotating group:
 C21(C22,C23,C24,C25,C26)
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_smtbx_masks_special_details
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A solvent mask was calculated and 1052 electrons were 
found in a volume of 3853\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
14[C3H7NO] per Asymmetric Unit 
which account for 1120 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38362
_shelx_hkl_checksum              92115
_shelx_fab_checksum              95590
_olex2_submission_special_instructions 'No special instructions were received'