Pure red-light emitting europium based complexes as efficient UV light converters: synthesis, crystal structure and photoluminescence properties.
Ali, Asgar; Ahmed, Zubair; Rahisuddin, ?; Iftikhar, K.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01536j

data_7714020
_publ_section_title
;
 Pure red-light emitting europium based complexes as efficient UV light
 converters: synthesis, crystal structure and photoluminescence
 properties.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01536j
_journal_year                    2023
_chemical_formula_moiety         'C42 H39 Eu F21 N3 O6, C Cl4'
_chemical_formula_sum            'C43 H39 Cl4 Eu F21 N3 O6'
_chemical_formula_weight         1386.53
_chemical_melting_point          456.5(15)
_chemical_name_common            'Europium-benzimidazole pyridine'
_chemical_name_systematic        '[Eu(fod)3(py-im)]'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-08 deposited with the CCDC.	2023-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.536(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1318(2)
_cell_length_b                   27.1014(4)
_cell_length_c                   15.0062(3)
_cell_measurement_reflns_used    31848
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.6600
_cell_measurement_theta_min      3.1860
_cell_volume                     5338.64(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_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    -13.00  70.22   0.38    2.21    --    5.68  67.00  83.00  219
  2  \w    -23.00   4.36   0.38    2.21    --   -5.52 -99.00 150.00   72
  3  \w    -64.00  18.08   0.38    2.21    --    5.68 -38.00 -30.00  216
  4  \w    -67.00  18.12   0.38    2.21    --    5.68 -67.00 -50.00  224
  5  \w    -22.00   8.02   0.38    2.21    --   -5.52 -99.00 -60.00   79
  6  \w    -23.00  14.24   0.38    2.21    --   -5.52 -99.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0329473000
_diffrn_orient_matrix_UB_12      -0.0191883000
_diffrn_orient_matrix_UB_13      0.0136097000
_diffrn_orient_matrix_UB_21      0.0343237000
_diffrn_orient_matrix_UB_22      -0.0057820000
_diffrn_orient_matrix_UB_23      0.0357983000
_diffrn_orient_matrix_UB_31      -0.0256170000
_diffrn_orient_matrix_UB_32      0.0168499000
_diffrn_orient_matrix_UB_33      0.0276986000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58918
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         3.104
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: carbon tetrachloride'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         13085
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0208P)^2^+10.5548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10903
_reflns_number_total             13085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01536j2.cif
_cod_data_source_block           eu-bmp
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '455 - 458' was changed to
'456.5(15)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7714020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H39 N2 O6 F21 Cl4 Eu1'
_chemical_oxdiff_usercomment     18-04-2023
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C43 \\sim Cl1A-C43A
 with sigma of 0.02
 Cl2-C43 \\sim Cl3A-C43A
 with sigma of 0.02
 Cl3-C43 \\sim Cl4A-C43A
 with sigma of 0.02
 Cl4-C43 \\sim Cl2A-C43A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl3A
 with sigma of 0.04
 Cl1-Cl3 \\sim Cl1A-Cl4A
 with sigma of 0.04
 Cl1-Cl4 \\sim Cl1A-Cl2A
 with sigma of 0.04
 Cl2-Cl3 \\sim Cl3A-Cl4A
 with sigma of 0.04
 Cl2-Cl4 \\sim Cl3A-Cl2A
 with sigma of 0.04
 Cl3-Cl4 \\sim Cl4A-Cl2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C43A)
4. Rigid body (RIGU) restrains
 Cl1, Cl1A, Cl2, Cl2A, Cl3, Cl3A, Cl4, Cl4A, C43, C43A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=Sof(C43A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(Cl4)=Sof(C43)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11),
 C18(H18), C28(H28), C38(H38)
6.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              36577
_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 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.732