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_7245668
_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         'C11 H9 N7 O2 Zn, C4 H9 N O'
_chemical_formula_sum            'C15 H18 N8 O3 Zn'
_chemical_formula_weight         423.74
_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             2022-09-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-07 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            4
_cell_length_a                   18.0312(5)
_cell_length_b                   11.2975(5)
_cell_length_c                   8.6680(3)
_cell_measurement_reflns_used    2671
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.1990
_cell_measurement_theta_min      4.6080
_cell_volume                     1765.74(11)
_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_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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     27.00  53.00   1.00    1.00    --   35.62-115.00 117.00   26
  2  \w    -27.00   6.00   1.00    1.00    --   35.62 -17.00 -61.00   33
  3  \w     80.00 158.00   1.00    1.41    --  107.12  17.00 107.00   78
  4  \w    116.00 143.00   1.00    1.41    --  107.12 117.00 -62.00   27
  5  \w     42.00  81.00   1.00    1.41    --  107.12-115.00 117.00   39
  6  \w   -101.00 -22.00   1.00    1.00    --  -35.62 -57.00  30.00   79
  7  \w     47.00  76.00   1.00    1.00    --   35.62-117.00-149.00   29
  8  \w     60.00 105.00   1.00    1.00    --   35.62 178.00-120.00   45
  9  \w    103.00 129.00   1.00    1.41    --  107.12 111.00 120.00   26
 10  \w    107.00 174.00   1.00    1.41    --  107.12  61.00   0.00   67
 11  \w     39.00 105.00   1.00    1.41    --  107.12 -95.00-150.00   66
 12  \w     57.00 123.00   1.00    1.41    --  107.12 -45.00-150.00   66
;
_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      0.0218319000
_diffrn_orient_matrix_UB_12      -0.1289020000
_diffrn_orient_matrix_UB_13      -0.0357796000
_diffrn_orient_matrix_UB_21      0.0816421000
_diffrn_orient_matrix_UB_22      0.0382058000
_diffrn_orient_matrix_UB_23      -0.0173565000
_diffrn_orient_matrix_UB_31      0.0126893000
_diffrn_orient_matrix_UB_32      -0.0229035000
_diffrn_orient_matrix_UB_33      0.1731585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4578
_diffrn_reflns_point_group_measured_fraction_full 0.698
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.529
_diffrn_reflns_theta_min         4.619
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70809
_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            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2338
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+2.0838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.296
_reflns_Friedel_fraction_full    0.352
_reflns_Friedel_fraction_max     0.332
_reflns_number_gt                2271
_reflns_number_total             2338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01092e2.cif
_cod_data_source_block           laq-1-20210420
_cod_database_code               7245668
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 C1 O1 N1'
_diffrn_oxdiff_digest_frames
;
01d2171d27f62fc9914e40beb8e95d0e4f000287742
;
_diffrn_oxdiff_digest_hkl
;
01fabc9ee0fc97588a3700c9cfb8cd1e91ab27
;
_reflns_odcompleteness_completeness 99.51
_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.a Rotating group:
 N2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C9(H9), C10(H10)
2.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              37323
_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 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.594