Fecht's acid revisited: a spirocyclic dicarboxylate for non-aromatic MOFs
Slyusarchuk, Valentyna D.; Hawes, Chris S.; CrystEngComm 24 (2022) 484–490; doi:10.1039/D1CE01542G

data_7243956
_publ_section_title
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 Fecht's acid revisited: a spirocyclic dicarboxylate for non-aromatic MOFs
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_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              484
_journal_page_last               490
_journal_paper_doi               10.1039/D1CE01542G
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C88 H104 N2 O38 Yb6, 1[C3H7NO], 1.5[H2O]'
_chemical_formula_sum            'C89.5 H112.5 N2.5 O41 Yb6'
_chemical_formula_weight         2917.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-18 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4079(8)
_cell_length_b                   20.8937(14)
_cell_length_c                   19.4442(12)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.75
_cell_volume                     5040.4(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50050
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.537
_diffrn_reflns_theta_min         2.095
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.598
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.6893.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_description       plate
_exptl_crystal_F_000             2830
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.502
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     640
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+88.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7129
_reflns_number_total             10423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01542g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7243956--7243957.cif.'
_cod_original_formula_sum        'C89.50 H112.50 N2.50 O41 Yb6'
_cod_database_code               7243956
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
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
2. Restrained distances
 C43-C40
 2.15 with sigma of 0.02
 C23-C22 = C21-C22 = C27-C22 = C27-C25 = C24-C25 = C24-C22
 1.53 with sigma of 0.02
 C25-C22
 2.15 with sigma of 0.02
 C42-C43 = C44-C43 = C44-C40 = C42-C40 = C39-C40 = C41-C40 = C38-C41 = C39-C38
 1.53 with sigma of 0.02
 C22-C20
 2.13 with sigma of 0.02
 C3-C2 = C5-C4 = C3-C4 = C5-C2 = C8-C4 = C7-C6 = C7-C8 = C6-C4
 1.53 with sigma of 0.02
 C4-C2
 2.15 with sigma of 0.02
 C29-C31
 2.15 with sigma of 0.02
 C30-C29 = C30-C31 = C32-C29 = C32-C31 = C35-C31 = C33-C34 = C33-C31 = C35-C34
 1.53 with sigma of 0.02
 C31-C34
 2.13 with sigma of 0.02
 C33-C35
 2.13 with sigma of 0.02
 C41-C39
 2.13 with sigma of 0.02
 C4-C7
 2.13 with sigma of 0.02
 O1-C1
 1.2 with sigma of 0.02
 C2-C1 \\sim C9-C7
 with sigma of 0.02
 C29-C28 \\sim C36-C34
 with sigma of 0.02
3. Restrained planarity
 O13, O14, C37, C38
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C34) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C37) = Uanis(C45)
Uanis(C1) = Uanis(C9)
Uanis(C28) = Uanis(C36)
5. Rigid body (RIGU) restrains
 O15, O16, O17, O18, C46, C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11, O12, C28, C29, C30, C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, O4, O5, O6, C10, C11, C12, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, O2, C1, C2, C3, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O13, O14, C37, C38, C39, C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C24, C25, C27, C22, C23, C20, C21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C1(0.5) C2(0.5) H2(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) C28(0.5) C29(0.5) H29(0.5) C30(0.5) H30A(0.5) H30B(0.5) C31(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) C37(0.5) C38(0.5) H38(0.5) C39(0.5)
 H39A(0.5) H39B(0.5) C40(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) C43(0.5) H43(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5)
7.a Ternary CH refined with riding coordinates:
 C11(H11), C16(H16), C20(H20), C25(H25), C47(H47), C52(H52), C2(H2), C7(H7),
 C29(H29), C34(H34), C38(H38), C43(H43)
7.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C21(H21A,
 H21B), C23(H23A,H23B), C24(H24A,H24B), C27(H27A,H27B), C48(H48A,H48B),
 C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C3(H3A,H3B), C5(H5A,H5B),
 C6(H6A,H6B), C8(H8A,H8B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B),
 C35(H35A,H35B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B)
7.c Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
7.d Aromatic/amide H refined with riding coordinates:
 C55(H55)
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_smtbx_masks_special_details
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A solvent mask was calculated and 104 electrons were found 
in a volume of 540\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[C3H7NO], 1.5[H2O] per Formula Unit 
which account for 110 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82146
_shelx_hkl_checksum              92126
_shelx_fab_checksum              97735
_olex2_submission_special_instructions 'No special instructions were received'