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_7245452
_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 Mn8 N4 O42 S8, 14[C3H7NO]'
_chemical_formula_sum            'C208 H164 Mn8 N4 O42 S8'
_chemical_formula_weight         4087.42
_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)
;
_audit_update_record
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2022-06-23 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.54
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.514
_cell_length_b                   22.114
_cell_length_c                   24.366
_cell_measurement_reflns_used    9405
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      59.01
_cell_measurement_theta_min      2.82
_cell_volume                     11963.439
_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 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.1151
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144863
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        59.332
_diffrn_reflns_theta_max         59.332
_diffrn_reflns_theta_min         1.990
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.494
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1556 before and 0.1004 after correction.
The Ratio of minimum to maximum transmission is 0.7342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       plate
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.790
_refine_diff_density_min         -2.353
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         16571
_refine_ls_number_restraints     2241
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.1467
_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^)+(0.0832P)^2^+383.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3197
_refine_ls_wR_factor_ref         0.3434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12232
_reflns_number_total             16571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00861k2.cif
_cod_data_source_block           eric525
_cod_original_cell_volume        11963.5
_cod_database_code               7245452
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.485
_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
 C7-C3 \\sim C17-C13 \\sim C27-C23 \\sim C37-C33
 with sigma of 0.02
 C17-C18 \\sim C17-C19 \\sim C17-C20
 with sigma of 0.02
 C27-C28 \\sim C27-C29 \\sim C27-C30
 with sigma of 0.02
 C18-C19 \\sim C19-C20 \\sim C20-C18
 with sigma of 0.02
 C7-C8 \\sim C7-C9 \\sim C7-C10
 with sigma of 0.02
 C37-C38 \\sim C37-C39 \\sim C37-C40
 with sigma of 0.02
 C28-C29 \\sim C29-C30 \\sim C30-C28
 with sigma of 0.02
 C38-C39 \\sim C39-C40 \\sim C40-C38
 with sigma of 0.02
 C8-C9 \\sim C9-C10 \\sim C10-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.0005 and sigma
for terminal atoms of 0.001 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
5.a 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), C52(H52), C49(H49), 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), C84(H84), C81(H81),
  C88(H88), C89(H89), C90(H90), C91(H91), C87(H87), C93(H93), C94(H94),
 C95(H95), C96(H96), C97(H97), C103(H103), C102(H102), C101(H101), C100(H100),
 C99(H99)
5.b Fitted hexagon refined as free rotating group:
 C6(C1,C2,C3,C4,C5), C16(C11,C12,C13,C14,C15), C26(C21,C22,C23,C24,C25),
 C35(C36,C31,C32,C33,C34), C42(C43,C44,C45,C46,C47), C53(C52,C51,C50,C49,C48),
 C55(C56,C57,C58,C59,C60), C61(C62,C63,C64,C65,C66), C67(C68,C69,C70,C71,C72),
 C74(C75,C76,C77,C78,C79), C85(C84,C83,C82,C81,C80), C88(C89,C90,C91,C92,C87),
 C93(C94,C95,C96,C97,C98), C103(C102,C101,C100,C99,C104)
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)
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_smtbx_masks_special_details
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A solvent mask was calculated and 1080 electrons were 
found in a volume of 3881\%A^3^ in 2 voids 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              30471
_shelx_hkl_checksum              2939
_shelx_fab_checksum              6951
_olex2_submission_special_instructions 'No special instructions were received'