A luminescent ytterbium(III)-organic framework for highly selective sensing of 2,4,6-trinitrophenol
Xin, Xuelian; Zhang, Minghui; Ji, Shijie; Dong, Hanxiao; Zhang, Liangliang; Journal of Solid State Chemistry 262 (2018) 186–190; doi:10.1016/j.jssc.2018.03.007

data_1561109
_publ_section_title
;
 A luminescent ytterbium(III)-organic framework for highly selective
 sensing of 2,4,6-trinitrophenol
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              186
_journal_page_last               190
_journal_paper_doi               10.1016/j.jssc.2018.03.007
_journal_volume                  262
_journal_year                    2018
_chemical_formula_moiety         'C24.5 H11.5 N3 O14 Yb2, H2 O'
_chemical_formula_sum            'C24.5 H13.5 N3 O15 Yb2'
_chemical_formula_weight         935.96
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5912(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.59404(20)
_cell_length_b                   14.31168(11)
_cell_length_c                   24.5365(2)
_cell_measurement_reflns_used    21165
_cell_measurement_temperature    107.43(10)
_cell_measurement_theta_max      70.5080
_cell_measurement_theta_min      3.6670
_cell_volume                     7823.18(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107.43(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -73.00 -14.00   1.00    7.50    --    0.00 149.00  90.00   59
  2  \w    -32.00  71.00   1.00    7.50    --    0.00  77.00 -30.00  103
  3  \w    -22.00  69.00   1.00    7.50    --    0.00  57.00-120.00   91
  4  \w     32.00 123.00   1.00    7.50    --   54.00  57.00  30.00   91
  5  \w      1.00  98.00   1.00    7.50    --   54.00 -99.00  90.00   97
  6  \w     23.00 112.00   1.00    7.50    --   54.00-125.00 -60.00   89
  7  \w     35.00 105.00   1.00    7.50    --   54.00  57.00-180.00   70
  8  \w     25.00  91.00   1.00    7.50    --   54.00-125.00 -90.00   66
  9  \w     -6.00  59.00   1.00    7.50    --   54.00 -57.00 -90.00   65
 10  \w      8.00 103.00   1.00    7.50    --   54.00  19.00-180.00   95
 11  \w    -15.00  17.00   1.00    7.50    --   54.00 -57.00-120.00   32
 12  \w     51.00 127.00   1.00    6.00    --  108.00 -50.00 -60.00   76
 13  \w     92.00 176.00   1.00    6.00    --  108.00  64.00 -30.00   84
 14  \w    113.00 172.00   1.00    6.00    --  108.00  25.00 -90.00   59
 15  \w     37.00 140.00   1.00    6.00    --  108.00 -77.00-150.00  103
 16  \w     41.00 112.00   1.00    6.00    --  108.00-111.00-150.00   71
 17  \w     90.00 115.00   1.00    6.00    --  108.00-111.00 -60.00   25
 18  \w     87.00 113.00   1.00    6.00    --  108.00-111.00  90.00   26
 19  \w     36.00 133.00   1.00    6.00    --  108.00 -38.00  30.00   97
 20  \w    106.00 132.00   1.00    6.00    --  108.00 111.00   0.00   26
 21  \w     72.00 104.00   1.00    6.00    --  108.00  25.00 -90.00   32
 22  \w     49.00 133.00   1.00    6.00    --  108.00 -38.00-180.00   84
 23  \w    101.00 127.00   1.00    6.00    --  108.00 111.00 -90.00   26
 24  \w     65.00 101.00   1.00    6.00    --  108.00-111.00  30.00   36
 25  \w     52.00 134.00   1.00    6.00    --  108.00 -77.00  30.00   82
 26  \w     49.00 129.00   1.00    6.00    --  108.00  12.00  90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124075000
_diffrn_orient_matrix_UB_12      0.0985186000
_diffrn_orient_matrix_UB_13      0.0245895000
_diffrn_orient_matrix_UB_21      0.0006983000
_diffrn_orient_matrix_UB_22      -0.0397024000
_diffrn_orient_matrix_UB_23      0.0584778000
_diffrn_orient_matrix_UB_31      0.0679994000
_diffrn_orient_matrix_UB_32      -0.0175527000
_diffrn_orient_matrix_UB_33      0.0057105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24355
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.67
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.131
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3532
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.593
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+429.7683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                6927
_reflns_number_total             6959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2018-262-186.cif
_cod_data_source_block           p
_cod_original_cell_volume        7823.18(12)
_cod_original_formula_sum        'C24.50 H13.50 N3 O15 Yb2'
_cod_database_code               1561109
_reflns_odcompleteness_completeness 99.90
_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:
 O2(H2A,H2B)
2.b Rotating group:
 O10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C3(H3), C4(H4), C13(H13), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C28(H28)
;