Adenine-based bio-MOFs with high water and acid–base stability for ammonia capture
Ruan, Mingming; Li, Anqi; Wen, Yaping; Zhou, Lian; Zhang, Jun; Xuan, Xiaopeng; CrystEngComm  (2022) –; doi:10.1039/D2CE01092E

data_7245667
_publ_section_title
;
 Adenine-based bio-MOFs with high water and acid--base stability for
 ammonia capture
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01092E
_journal_year                    2022
_chemical_formula_moiety         '0.5(C48 H40 N24 O8 Zn4), C3 H7 N O'
_chemical_formula_sum            'C27 H27 N13 O5 Zn2'
_chemical_formula_weight         744.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-10 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6657(3)
_cell_length_b                   11.3205(2)
_cell_length_c                   8.8645(2)
_cell_measurement_reflns_used    3427
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3310
_cell_measurement_theta_min      6.3310
_cell_volume                     1772.76(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -94.00  -7.00   1.00    1.00    --  -35.62 133.00-140.00   87
  2  \w    -54.00  18.00   1.00    1.00    --  -35.62  62.00 163.00   72
  3  \w    106.00 132.00   1.00    3.17    --  107.12  62.00 163.00   26
  4  \w     41.00 122.00   1.00    3.17    --  107.12 -62.00  25.00   81
  5  \w     90.00 118.00   1.00    3.17    --  107.12 -58.00-154.00   28
  6  \w    106.00 173.00   1.00    3.17    --  107.12  58.00 -13.00   67
  7  \w     44.00 102.00   1.00    3.17    --  107.12-136.00 -26.00   58
  8  \w      1.00  70.00   1.00    1.00    --   35.62 -99.00 150.00   69
  9  \w     36.00  94.00   1.00    1.00    --   35.62  57.00-150.00   58
 10  \w    101.00 177.00   1.00    3.17    --  107.12 111.00 -60.00   76
 11  \w     91.00 172.00   1.00    3.17    --  107.12  45.00-120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0061129000
_diffrn_orient_matrix_UB_12      -0.1355396000
_diffrn_orient_matrix_UB_13      0.0098426000
_diffrn_orient_matrix_UB_21      0.0601561000
_diffrn_orient_matrix_UB_22      -0.0122008000
_diffrn_orient_matrix_UB_23      -0.1247868000
_diffrn_orient_matrix_UB_31      0.0627772000
_diffrn_orient_matrix_UB_32      -0.0015317000
_diffrn_orient_matrix_UB_33      0.1206682000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5570
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.552
_diffrn_reflns_theta_min         4.639
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yelllow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 888 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2800
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.657
_reflns_Friedel_fraction_max     0.622
_reflns_number_gt                2665
_reflns_number_total             2800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01092e2.cif
_cod_data_source_block           laq-20210407
_cod_database_code               7245667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 C1 N1 '
_diffrn_oxdiff_digest_frames
;
01b45756eacbcdfda39eef6f0ea20d2d2800036a905
;
_diffrn_oxdiff_digest_hkl
;
01333283307af2f7efd5972a2c719ca95b2f98
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C13 = O4-C17
 1.2 with sigma of 0.01
 O3-N7
 2.2 with sigma of 0.02
 N8-C17 = N7-C13 = N7-C14 = N8-C16 = N8-C18 = N7-C15
 1.48 with sigma of 0.01
 C15-C14 = C16-C18
 2.5 with sigma of 0.02
 C16-C17
 2.5 with sigma of 0.02
 C13-C15
 2.5 with sigma of 0.02
3. Restrained planarity
 C14, N7, C13, C15, O3
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C15 \\sim N7 \\sim C13 \\sim C14 \\sim O3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N7 \\sim O3 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim N8 \\sim C17 \\sim
C18 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N7) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N8) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C15, N7, C13, C14, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, O3, C13, C14, C15, C16, N8, C17, C18, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(N8)=Sof(C17)=Sof(H17)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O4)=0.5*(1-FVAR(2))
 Sof(N7)=Sof(O3)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=0.5*FVAR(2)
7.a Rotating group:
 N6(H6A,H6B)
7.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C13(H13), C17(H17)
;
_shelx_res_checksum              22462
_olex2_date_sample_data_collection 2021-04-07
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.576