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_7243957
_publ_section_title
;
 Fecht's acid revisited: a spirocyclic dicarboxylate for non-aromatic MOFs
;
_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
'C21 H20 N2 O4 Zn, 1.3333[C3H7NO], 1.3333[H2O]'
_chemical_formula_sum            'C25 H32 N3.33 O6.67 Zn'
_chemical_formula_weight         551.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3429(10)
_cell_length_b                   12.4311(10)
_cell_length_c                   18.5115(14)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.476
_cell_measurement_theta_min      2.668
_cell_volume                     2610.2(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.990
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15765
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         3.278
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0696 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.7919.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1155
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2688
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0688P)^2^+3.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1849
_reflns_number_total             2688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01542g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7243956--7243957.cif.'
_cod_database_code               7243957
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C6-C8
 2.2 with sigma of 0.02
 C7-C4 \\sim C4-C2
 with sigma of 0.02
 C9-C7 \\sim C2-C1
 with sigma of 0.02
 O4-C9 \\sim O3-C9 \\sim O2-C1 \\sim O1-C1
 with sigma of 0.02
 C6-C4 \\sim C8-C4 \\sim C5-C4 \\sim C3-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C9)
Uanis(O3) = Uanis(O1)
4. Rigid body (RIGU) restrains
 C4, C1, C2, C3, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5) C1(0.5) C2(0.5) H2(0.5) C3(0.5)
 H3A(0.5) H3B(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) C9(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C14(H14), C15(H15)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 172 electrons were 
found in a volume of 838\%A^3^ in 1 void per unit cell. 
Supporting methods suggest 1.333[C3H7NO], 1.333[H2O] per 
Formula Unit in the bulk material which account for 266 
electrons per unit cell. The solvation in an individual
crystal may be somewhat lower.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80487
_shelx_hkl_checksum              60302
_shelx_fab_checksum              96914
_olex2_submission_special_instructions 'No special instructions were received'