Mixed-Lanthanide Porous Coordination Polymers Showing Range-Tunable Ratiometric Luminescence for O2 Sensing.
Ye, Jia-Wen; Lin, Jiao-Min; Mo, Zong-Wen; He, Chun-Ting; Zhou, Hao-Long; Zhang, Jie-Peng; Chen, Xiao-Ming; Inorganic chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00252

data_4345923
_publ_section_title
;
 Mixed-Lanthanide Porous Coordination Polymers Showing Range-Tunable
 Ratiometric Luminescence for O2 Sensing.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00252
_journal_year                    2017
_chemical_formula_moiety         '0.25(C92 H56 N12 O24 Tb4)'
_chemical_formula_sum            'C23 H14 N3 O6 Tb'
_chemical_formula_weight         587.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3440(2)
_cell_length_b                   8.29446(13)
_cell_length_c                   23.7201(5)
_cell_measurement_reflns_used    13131
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.8450
_cell_measurement_theta_min      3.6990
_cell_volume                     2428.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_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   -107.00 -18.00   1.00   28.00    --  -32.00 -72.00 108.00   89
  2  \w    -78.00 -18.00   1.00   28.00    --  -32.00 -72.00-180.00   60
  3  \w    -47.00  14.00   1.00   28.00    --  -32.00  72.00  36.00   61
  4  \w    -47.00  50.00   1.00   28.00    --  -32.00  72.00-180.00   97
  5  \w    -78.00 -18.00   1.00   28.00    --  -32.00 -72.00  36.00   60
  6  \w    -47.00  14.00   1.00   28.00    --  -32.00  72.00 108.00   61
  7  \w    -78.00 -18.00   1.00   28.00    --  -32.00 -72.00-108.00   60
  8  \w    -47.00  15.00   1.00   28.00    --  -32.00  72.00 -36.00   62
  9  \w   -146.00 -20.00   1.00   65.00    -- -110.00   0.00  36.00  126
 10  \w   -120.00 -52.00   1.00   65.00    -- -110.00  72.00-108.00   68
 11  \w   -124.00 -64.00   1.00   65.00    -- -110.00  72.00-180.00   60
 12  \w   -200.00-139.00   1.00   65.00    -- -110.00 -72.00 -36.00   61
 13  \w   -115.00 -55.00   1.00   65.00    -- -110.00  72.00 108.00   60
 14  \w   -125.00 -20.00   1.00   65.00    -- -110.00  72.00 -36.00  105
 15  \w   -189.00 -80.00   1.00   65.00    -- -110.00   0.00-180.00  109
 16  \w    -98.00 -38.00   1.00   65.00    -- -110.00  72.00  36.00   60
 17  \w   -200.00-139.00   1.00   65.00    -- -110.00 -72.00  36.00   61
 18  \w   -200.00-123.00   1.00   65.00    -- -110.00 -72.00-108.00   77
 19  \w   -200.00-119.00   1.00   65.00    -- -110.00 -72.00-180.00   81
 20  \w   -200.00 -96.00   1.00   65.00    -- -110.00 -72.00 108.00  104
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21472
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.478
_diffrn_reflns_theta_min         3.581
_exptl_absorpt_coefficient_mu    14.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
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    1.606
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00047(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+3.8600P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2388
_reflns_number_total             2599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00252_si_002.cif
_cod_data_source_block           mcf-53(tb)
_cod_database_code               4345923
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{N2, C8}
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C8)
4. Others
 Fixed Sof: O4(0.5) C1(0.5) H1(0.5) C8(0.5) H8(0.5) H14A(0.5) H14(0.5)
 H1A(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14A),
 C14(H14), N1(H1A)
;
_shelx_res_checksum              82579
_shelx_hkl_checksum              73805
_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
- Detector area scaling
;