Structure and properties of metal-organic frameworks precisely modulated by sulfate ion
Guo, Yuanyuan; Wang, Ruidong; Wei, Wei-Ming; Fang, Fang; Zhao, Xu-Hui; Zhang, Suo-Shu; Shen, Tian-Ze; Zhang, Jun; Zhao, Qi-Hua; Wang, Juan; Dalton Transactions  (2023) –; doi:10.1039/D3DT01995K

data_7714151
_publ_section_title
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 Structure and properties of metal-organic frameworks precisely modulated
 by sulfate ion
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01995K
_journal_year                    2023
_chemical_formula_moiety         'C76 H60 Cd3 N16 O14 S3, 2(H2 O), 10[H2O]'
_chemical_formula_sum            'C76 H84 Cd3 N16 O26 S3'
_chemical_formula_weight         2071.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-09-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2023-09-04 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.060(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.054(3)
_cell_length_b                   9.6261(9)
_cell_length_c                   31.428(3)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.21
_cell_volume                     9517.2(16)
_computing_data_collection       SMART(Bruker,2000)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0899
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            87230
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.377
_diffrn_reflns_theta_min         2.019
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6410
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1138 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.8596.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            CHARTREUSE
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11889
_refine_ls_number_restraints     340
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0845P)^2^+129.8134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8873
_reflns_number_total             11889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01995k2.cif
_cod_data_source_block           2
_cod_original_cell_volume        9516.9(14)
_cod_database_code               7714151
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Restrained distances
 S2-O6 = S2-O3 = S2-O11 = S2-O14
 1.45 with sigma of 0.01
 S1-O1 = S1-O12 = S1-O8 = S1-O4
 1.45 with sigma of 0.01
 O4-O12 \\sim O12-O1
 with sigma of 0.01
 O1-O12 \\sim O12-O8
 with sigma of 0.01
 O4-O12 \\sim O12-O8
 with sigma of 0.01
 O4-O1 \\sim O1-O8
 with sigma of 0.01
 O1-O8 \\sim O7-O9
 with sigma of 0.04
 O4-O8 \\sim O2-O9
 with sigma of 0.04
 Cd2-O1 \\sim Cd2-O7
 with sigma of 0.02
 O8-O12 \\sim O9-O5
 with sigma of 0.04
 S1-O1 \\sim S1A-O7
 with sigma of 0.02
 S1-O4 \\sim S1A-O2
 with sigma of 0.02
 O1-O4 \\sim O7-O2
 with sigma of 0.04
 O1-O12 \\sim O7-O5
 with sigma of 0.04
 S1-O12 \\sim S1A-O5
 with sigma of 0.02
 O4-O12 \\sim O2-O5
 with sigma of 0.04
 S1-O8 \\sim S1A-O9
 with sigma of 0.02
 Cd2-S1 \\sim Cd2-S1A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
S1 \\sim O1 \\sim O4 \\sim O8 \\sim O12 \\sim O7 \\sim S1A \\sim O2 \\sim O9
\\sim O5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
S2 \\sim O6 \\sim O14 \\sim O11 \\sim O3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(S1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O12) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
3. Rigid body (RIGU) restrains
 Cd2, S2, S1, O1, O4, O6, O8, O10, O12, O14
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0001
 S1, O1, O4, O8, O12, O7, S1A, O2, O9, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S2, O6, O14, O11, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(O7)=Sof(S1A)=Sof(O2)=Sof(O9)=Sof(O5)=1-FVAR(1)
 Sof(S1)=Sof(O1)=Sof(O4)=Sof(O8)=Sof(O12)=FVAR(1)
 Fixed Sof: S2(0.5) O6(0.5) O14(0.5) O11(0.5) O3(0.5)
5.a Riding coordinates:
 O10(H10A,H10B), O13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C34(H34), C32(H32), C37(H37), C24(H24), C3(H3), C22(H22), C23(H23),
 C15(H15), C27(H27), C33(H33), C25(H25), C9(H9), C29(H29), C31(H31), C38(H38),
 C14(H14), C28(H28), C36(H36), C18(H18), C17(H17), C16(H16), C11(H11), C6(H6),
 C12(H12), C1(H1), C2(H2), C5(H5)
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_smtbx_masks_special_details
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A solvent mask was calculated and 820 electrons were 
found in a volume of 2628\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
20[H2O] per Asymmetric Unit 
which account for 800 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52795
_shelx_fab_checksum              10457
_olex2_submission_special_instructions 'No special instructions were received'