Eu3+/Tb3+ and Dy3+ POM@MOFs and 2D coordination polymers based on pyridine-2,6-dicarboxylic acid for ratiometric optical temperature sensing
Kaczmarek, Anna M.; Journal of Materials Chemistry C 6 (2018) 5916–; doi:10.1039/C8TC01062E

data_7237302
_publ_section_title
;
 Eu3+/Tb3+ and Dy3+ POM@MOFs and 2D coordination polymers based on
 pyridine-2,6-dicarboxylic acid for ratiometric optical temperature
 sensing
;
_journal_issue                   22
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              5916
_journal_paper_doi               10.1039/C8TC01062E
_journal_volume                  6
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H12 La4 N4 O32, Mo12 O40 Si, 2(O)'
_chemical_formula_sum            'C28 H12 La4 Mo12 N4 O74 Si'
_chemical_formula_weight         3323.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-14
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.948(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4498(4)
_cell_length_b                   15.6306(2)
_cell_length_c                   22.1378(3)
_cell_measurement_reflns_used    14152
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.3780
_cell_measurement_theta_min      3.1660
_cell_volume                     7758.0(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.969
_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     25.00  90.00   1.00   30.00    --   10.33-165.00  72.00   65
  2  \w     20.00  50.00   1.00   30.00    --   10.33-116.00-140.00   30
  3  \w    -46.00  38.00   1.00   30.00    --   10.33 -57.00 -60.00   84
  4  \w     -6.00  40.00   1.00   30.00    --   10.33  38.00 -30.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0034103000
_diffrn_orient_matrix_UB_12      0.0426102000
_diffrn_orient_matrix_UB_13      -0.0102369000
_diffrn_orient_matrix_UB_21      -0.0200751000
_diffrn_orient_matrix_UB_22      -0.0085477000
_diffrn_orient_matrix_UB_23      -0.0250555000
_diffrn_orient_matrix_UB_31      -0.0242462000
_diffrn_orient_matrix_UB_32      0.0130252000
_diffrn_orient_matrix_UB_33      0.0171546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20420
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.162
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.845
_exptl_crystal_description       block
_exptl_crystal_F_000             6184
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.089
_refine_diff_density_max         5.194
_refine_diff_density_min         -1.827
_refine_diff_density_rms         0.254
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         11228
_refine_ls_number_restraints     1853
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0751P)^2^+149.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                10807
_reflns_number_total             11228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc01062e2.cif
_cod_data_source_block           la_pdc_mo12o40si
_cod_database_code               7237302
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H12 La4 Mo12 N4 O74 Si'
_reflns_odcompleteness_completeness 95.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.88(2)
 0.12(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.002 and
sigma for terminal atoms of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              92874
_shelx_hkl_checksum              89615
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.782