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_7714150
_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 H60.8 Cd3 N16 O8.8 S1.6, 1.4(H2 O2),6.2(H2O)'
_chemical_formula_sum            'C76 H76 Cd3 N16 O17.8 S1.6'
_chemical_formula_weight         1886.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 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                 100.727(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.694(3)
_cell_length_b                   9.6200(8)
_cell_length_c                   16.0832(13)
_cell_measurement_reflns_used    4534
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.22
_cell_volume                     4818.0(7)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       SMART(Bruker,2000)
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20276
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.477
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8866.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(7)
_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     589
_refine_ls_number_reflns         9050
_refine_ls_number_restraints     609
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1372P)^2^+8.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2421
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.860
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                6160
_reflns_number_total             9050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01995k2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C76 H76 Cd3 N16 O17.80 S1.60'
_cod_database_code               7714150
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98241
 0.01759
2. Restrained distances
 O6-O7 = O5-O8
 2.4 with sigma of 0.01
 O7-O5
 2.4 with sigma of 0.01
 O7-O8
 2.4 with sigma of 0.01
 O6-O5
 2.4 with sigma of 0.01
 O6-O8
 2.4 with sigma of 0.01
 O5-Cd2
 2.2 with sigma of 0.01
 S2-O6 = S2-O5 = S2-O8 = S2-O7
 1.3 with sigma of 0.01
 Cd2-H1A \\sim Cd2-H1B
 with sigma of 0.02
 N7-C3 \\sim N9-C39
 with sigma of 0.02
 N7-C5 \\sim N9-C41
 with sigma of 0.02
 N7-C17 \\sim N9-C17
 with sigma of 0.02
 C3-C4 \\sim C39-C40
 with sigma of 0.02
 C4-N8 \\sim C40-N10
 with sigma of 0.02
 N8-C5 \\sim N10-C41
 with sigma of 0.02
 N7-C4 \\sim N9-C40
 with sigma of 0.04
 N7-N8 \\sim N9-N10
 with sigma of 0.04
 C3-N8 \\sim C39-N10
 with sigma of 0.04
 C3-C5 \\sim C39-C41
 with sigma of 0.04
 C3-C17 \\sim C39-C17
 with sigma of 0.04
 C4-C5 \\sim C40-C41
 with sigma of 0.04
 C5-C17 \\sim C41-C17
 with sigma of 0.04
 C15-N9 \\sim N9-C35
 with sigma of 0.01
 C15-N7 \\sim N7-C35
 with sigma of 0.01
3. Restrained planarity
 C39, C41, N9, C17
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
S4 \\sim O13 \\sim O14 \\sim O15 \\sim O16: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N7 \\sim C3 \\sim C4 \\sim N8 \\sim C5 \\sim C39 \\sim C40 \\sim N10 \\sim C41
\\sim N9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O5 \\sim O6 \\sim O7 \\sim S2 \\sim O8: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C1 \\sim C24 \\sim C35 \\sim C17 \\sim C15 \\sim C25: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O4) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(S4) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N8) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(N10) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(S2) \\sim
Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C38) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 S4, O13, O14, O15, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C3, C4, N8, C5, C39, C40, N10, C41, N9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, O6, O7, S2, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S2, O7, O6, O8, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C24, C35, C17, C15, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(N10)=Sof(C41)=Sof(H41)=Sof(N9)=1-
 FVAR(1)
 Sof(N7)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(N8)=Sof(C5)=Sof(H5)=FVAR(1)
 Fixed Sof: O5(0.3) O6(0.3) O7(0.3) S2(0.3) O8(0.3) S4(0.5) O13(0.5) O14(0.5)
 O15(0.5) O16(0.5) O1(0.7) H1A(0.7) H1B(0.7) O2(0.5) H2A(0.5) H2B(0.5) H3A(0.5)
 O4(0.5) H4A(0.5) O9(0.4) H9A(0.4)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A), O4(H4A), O9(H9A)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
7.c Fitted pentagon refined as free rotating group:
 N7(C3,C4,N8,C5), C39(C40,N10,C41,N9)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 354 electrons were 
found in a volume of 1552\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 18[H2O] per Formula Unit 
which account for 360 electrons per unit cell.
;
_shelx_res_checksum              82327
_shelx_fab_checksum              32262
_olex2_submission_special_instructions 'No special instructions were received'