Solvent-induced terbium metal-organic frameworks for highly selective detection of manganese(ii) ions.
Wang, Yutong; Wang, Xia; Zhang, Kailiang; Wang, Xiaokang; Xin, Xuelian; Fan, Weidong; Dai, Fangna; Han, Yinfeng; Sun, Daofeng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2569–2573; doi:10.1039/c9dt00006b

data_7048728
_publ_section_title
;
 Solvent-induced terbium metal-organic frameworks for highly selective
 detection of manganese(ii) ions.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2569
_journal_page_last               2573
_journal_paper_doi               10.1039/c9dt00006b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C33 H27 N O17 S6 Tb2, H2 O'
_chemical_formula_sum            'C33 H29 N O18 S6 Tb2'
_chemical_formula_weight         1237.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                69.310(4)
_cell_angle_beta                 83.274(4)
_cell_angle_gamma                83.634(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9253(5)
_cell_length_b                   13.7830(6)
_cell_length_c                   16.2197(8)
_cell_measurement_reflns_used    10259
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      70.4400
_cell_measurement_theta_min      4.4830
_cell_volume                     2055.70(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.877
_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    -69.00  22.00   1.00    1.13    --    0.00 -57.00 -90.00   91
  2  \w    -42.00  24.00   1.00    1.13    --    0.00  96.00 114.00   66
  3  \w    -22.00  69.00   1.00    1.13    --    0.00  57.00  60.00   91
  4  \w     22.00 125.00   1.00    4.50    --   54.00  77.00 -30.00  103
  5  \w     22.00 125.00   1.00    4.50    --   54.00  77.00   0.00  103
  6  \w     32.00 123.00   1.00    4.50    --   54.00  57.00  60.00   91
  7  \w    -15.00  76.00   1.00    4.50    --   54.00 -57.00 150.00   91
  8  \w     22.00 125.00   1.00    4.50    --   54.00  77.00 -90.00  103
  9  \w     23.00 112.00   1.00    4.50    --   54.00-125.00 120.00   89
 10  \w     32.00 123.00   1.00    4.50    --   54.00  57.00-180.00   91
 11  \w      1.00  98.00   1.00    4.50    --   54.00 -99.00 150.00   97
 12  \w    100.00 178.00   1.00    4.50    --  108.00 111.00 -30.00   78
 13  \w     35.00 135.00   1.00    4.50    --  108.00 -38.00-150.00  100
 14  \w     85.00 178.00   1.00    4.50    --  108.00  50.00  30.00   93
 15  \w     84.00 175.00   1.00    4.50    --  108.00  63.00-150.00   91
 16  \w    100.00 178.00   1.00    4.50    --  108.00 111.00  60.00   78
 17  \w     57.00 151.00   1.00    4.50    --  108.00 178.00  90.00   94
 18  \w     35.00 112.00   1.00    4.50    --  108.00-111.00-180.00   77
 19  \w     37.00 140.00   1.00    4.50    --  108.00 -77.00  60.00  103
 20  \w     35.00 112.00   1.00    4.50    --  108.00-111.00 -90.00   77
 21  \w     37.00 131.00   1.00    4.50    --  108.00 -50.00 -30.00   94
 22  \w     34.00 178.00   1.00    4.50    --  108.00   0.00-180.00  144
 23  \w     35.00 112.00   1.00    4.50    --  108.00-111.00 -60.00   77
 24  \w     35.00 135.00   1.00    4.50    --  108.00 -38.00  60.00  100
 25  \w     35.00 112.00   1.00    4.50    --  108.00-111.00  60.00   77
 26  \w    -27.00  73.00   1.00    1.13    --    0.00  38.00 -30.00  100
 27  \w    -32.00  71.00   1.00    1.13    --    0.00  77.00 -30.00  103
 28  \w    -74.00  49.00   1.00    1.13    --    0.00 -19.00  30.00  123
 29  \w     22.00 125.00   1.00    4.50    --   54.00  77.00-150.00  103
 30  \w    -15.00  76.00   1.00    4.50    --   54.00 -57.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0530937000
_diffrn_orient_matrix_UB_12      -0.1132267000
_diffrn_orient_matrix_UB_13      0.0478758000
_diffrn_orient_matrix_UB_21      -0.0960967000
_diffrn_orient_matrix_UB_22      -0.0024237000
_diffrn_orient_matrix_UB_23      0.0823832000
_diffrn_orient_matrix_UB_31      -0.1118513000
_diffrn_orient_matrix_UB_32      -0.0391064000
_diffrn_orient_matrix_UB_33      -0.0360840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.850
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19458
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         70.764
_diffrn_reflns_theta_min         3.665
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_refine_diff_density_max         2.387
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0743P)^2^+16.1214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5921
_reflns_number_total             6928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00006b2.cif
_cod_data_source_block           UPC-36
_cod_depositor_comments
'Adding full bibliography for 7048728--7048729.cif.'
_cod_database_code               7048728
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N S Tb'
_reflns_odcompleteness_completeness 99.97
_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 C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O17(H17A,H17B)
2.b Rotating group:
 O6(H6A,H6B), O6AA(H6AA,H6AB), O10(H10A,H10B), O9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C12(H12), C22(H22), C25(H25), C26(H26), C33(H33), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C9(H9)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              50714
_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 1.951
_oxdiff_exptl_absorpt_empirical_full_min 0.591