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_7245453
_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
'C208 H164 Mg8 N4 O42 S8, 2(C2 H8 N), 4(C3 H7 N O), 2[C3H7NO], 2[C3H7NO]'
_chemical_formula_sum            'C236 H236 Mg8 N14 O50 S8'
_chemical_formula_weight         4519.33
_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             2021-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                80.495(3)
_cell_angle_beta                 88.866(3)
_cell_angle_gamma                76.732(3)
_cell_formula_units_Z            1
_cell_length_a                   13.6310(8)
_cell_length_b                   19.4305(11)
_cell_length_c                   22.6660(14)
_cell_measurement_reflns_used    9160
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      50.51
_cell_measurement_theta_min      3.33
_cell_volume                     5761.8(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            103137
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        50.578
_diffrn_reflns_theta_max         50.578
_diffrn_reflns_theta_min         2.369
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1311 before and 0.0870 after correction.
The Ratio of minimum to maximum transmission is 0.8809.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             2374
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.156
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1179
_refine_ls_number_reflns         11619
_refine_ls_number_restraints     1026
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.1115
_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^)+(0.0531P)^2^+102.8625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2602
_refine_ls_wR_factor_ref         0.2641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10521
_reflns_number_total             11619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00861k2.cif
_cod_data_source_block           eric526
_cod_database_code               7245453
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C13 \\sim C7-C3 \\sim C28-C23 \\sim C37-C33
 with sigma of 0.02
 C39-C37 \\sim C40-C37 \\sim C38-C37 \\sim C31-C28 \\sim C29-C28 \\sim C30-C28
\\sim C9-C7 \\sim C8-C7 ~
 C7-C10 \\sim C19-C17 \\sim C20-C17 \\sim C18-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004 within 2A
Uanis(O1_4) = Uanis(O1_5)
Uanis(N1_4) = Uanis(N1_5)
Uanis(C1_4) = Uanis(C1_5)
Uanis(C2_4) = Uanis(C2_5)
Uanis(C3_4) = Uanis(C3_5)
4. Others
 Sof(O1)=Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(O1)=Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Free rotating group:
 O1(N1,C1,C2,C3), O1(N1,C1,C2,C3)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C12(H12), C14(H14), C22(H22), C24(H24), C32(H32), C34(H34),
 C43(H43), C46(H46), C49(H49), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67),
 C68(H68), C69(H69), C70(H70), C71(H71), C75(H75), C78(H78), C81(H81), C84(H84),
  C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C93(H93), C94(H94),
 C95(H95), C96(H96), C97(H97), C99(H99), C100(H100), C101(H101), C102(H102),
 C103(H103), C1(H1), C1(H1), C1(H1)
5.e Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C11(C12,C13,C14,C15,C16), C21(C22,C23,C24,C25,C26),
 C27(C32,C33,C34,C35,C36), C42(C43,C44,C45,C46,C47), C48(C49,C50,C51,C52,C53),
 C55(C56,C57,C58,C59,C60), C61(C62,C63,C64,C65,C66), C67(C68,C69,C70,C71,C72),
 C74(C75,C76,C77,C78,C79), C80(C81,C82,C83,C84,C85), C87(C88,C89,C90,C91,C92),
 C93(C94,C95,C96,C97,C98), C99(C100,C101,C102,C103,C104)
5.f 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), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C1(H1C,H1D,H1E), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 165 electrons were 
found in a volume of 779\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
2[C3H7NO], 2[C3H7NO] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27222
_shelx_hkl_checksum              98944
_shelx_fab_checksum              10491
_olex2_submission_special_instructions 'No special instructions were received'