Heterometallic organic framework: A highly selective functional probe for carmine and TNP molecules
Wu, Nan; Li, Zhang; Jia, Yuejiao; Li, Dechao; Hu, Ming; CrystEngComm  (2022) –; doi:10.1039/D2CE01417C

data_7245809
_publ_section_title
;
 Heterometallic organic framework: A highly selective functional probe for
 carmine and TNP molecules
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01417C
_journal_year                    2022
_chemical_formula_moiety         'C25 H19 N4 O13 Tb Zn, 2(H2 O)'
_chemical_formula_sum            'C25 H23 N4 O15 Tb Zn'
_chemical_formula_weight         843.76
_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             2022-07-20
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-07-27 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6321(2)
_cell_length_b                   12.56880(10)
_cell_length_c                   18.42700(10)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    300.69(10)
_cell_measurement_theta_max      73.2960
_cell_measurement_theta_min      3.7110
_cell_volume                     5529.83(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.69(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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    -38.00  19.00   0.50    0.93    --    0.00  77.00   0.00  114
  2  \w     -6.00  37.00   0.50    0.93    --    0.00 -57.00 -60.00   86
  3  \w    -88.00 -22.00   0.50    0.93    --    0.00 -57.00 -60.00  132
  4  \w    115.00 168.00   0.50    3.71    --   98.20  82.00 -90.00  106
  5  \w     95.00 121.00   0.50    3.71    --   98.20 -82.00  90.00   52
  6  \w     63.00 133.00   0.50    3.71    --   98.20 -82.00 120.00  140
  7  \w     67.00 111.00   0.50    3.71    --   98.20  82.00 -90.00   88
  8  \w     91.00 117.00   0.50    3.71    --   98.20  61.00  60.00   52
  9  \w    134.00 180.00   0.50    3.71    --   98.20  61.00  60.00   92
 10  \w     10.00 125.00   0.50    3.71    --   98.20 -77.00   0.00  230
 11  \w     83.00 187.00   0.50    3.71    --   98.20  61.00-150.00  208
 12  \w     84.00 125.00   0.50    3.71    --   98.20 -82.00-180.00   82
 13  \w     68.00 136.00   0.50    3.71    --   98.20  82.00 120.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0108312000
_diffrn_orient_matrix_UB_12      -0.1106255000
_diffrn_orient_matrix_UB_13      -0.0296441000
_diffrn_orient_matrix_UB_21      -0.0091675000
_diffrn_orient_matrix_UB_22      -0.0515104000
_diffrn_orient_matrix_UB_23      0.0718543000
_diffrn_orient_matrix_UB_31      -0.0629703000
_diffrn_orient_matrix_UB_32      -0.0114801000
_diffrn_orient_matrix_UB_33      -0.0373213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13913
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.487
_diffrn_reflns_theta_min         3.703
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.342
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0363P)^2^+5.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5031
_reflns_number_total             5408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01417c2.cif
_cod_data_source_block           lz-2
_cod_database_code               7245809
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.280
_shelx_estimated_absorpt_t_min   0.092
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B)
2.b Rotating group:
 O8(H8A,H8B), O5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C21(H21), C22(H22), C4(H4), C14(H14), C19(H19), C13(H13), C7(H7),
 C2(H2), C1(H1), C9(H9), C10(H10), C25(H25)
;
_shelx_res_checksum              87773
_shelx_hkl_checksum              61794
_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 2.204
_oxdiff_exptl_absorpt_empirical_full_min 0.719