Enhanced circularly polarized luminescence of chiral Eu(III) coordination polymers with structural strain.
Tsurui, Makoto; Kitagawa, Yuichi; Shoji, Sunao; Fushimi, Koji; Hasegawa, Yasuchika; Dalton transactions (Cambridge, England : 2003) 52 (2023) 796–805; doi:10.1039/d2dt03422k

data_7711917
_publ_section_title
;
 Enhanced circularly polarized luminescence of chiral Eu(III) coordination
 polymers with structural strain.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              796
_journal_page_last               805
_journal_paper_doi               10.1039/d2dt03422k
_journal_volume                  52
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C73 H66 Eu F15 O8 P2'
_chemical_formula_sum            'C73 H66 Eu F15 O8 P2'
_chemical_formula_weight         1570.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-17 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7325(3)
_cell_length_b                   19.2862(3)
_cell_length_c                   21.0290(3)
_cell_measurement_reflns_used    30980
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      30.3890
_cell_measurement_theta_min      2.1080
_cell_volume                     7191.76(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.795
_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    -80.00   0.00   0.50   42.81    --   -5.96 -20.00 149.00  160
  2  \w    -17.00  28.00   0.50   42.81    --   -5.96 -99.00  90.00   90
  3  \w    -15.00  70.00   0.50   42.81    --   -5.96  20.00 -43.00  170
  4  \w      5.00  30.00   0.50   42.81    --   -5.96  19.00-180.00   50
  5  \w     -1.00  28.00   0.50   42.81    --   -5.96 -99.00 -90.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0289006000
_diffrn_orient_matrix_UB_12      -0.0247329000
_diffrn_orient_matrix_UB_13      0.0052564000
_diffrn_orient_matrix_UB_21      0.0257137000
_diffrn_orient_matrix_UB_22      0.0271566000
_diffrn_orient_matrix_UB_23      0.0070012000
_diffrn_orient_matrix_UB_31      -0.0101442000
_diffrn_orient_matrix_UB_32      -0.0018295000
_diffrn_orient_matrix_UB_33      0.0325814000
_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  0.0806
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.082
_diffrn_reflns_theta_min         1.836
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 5673 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         17870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0922P)^2^+6.1211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.750
_reflns_number_gt                15079
_reflns_number_total             17870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03422k2.cif
_cod_data_source_block           '[Eu(+pfc)3(p-dpeb)]n'
_cod_depositor_comments
'Adding full bibliography for 7711917--7711918.cif.'
_cod_database_code               7711917
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Eu C H O P F'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C41(H41), C58(H58), C78(H78)
2.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B), C40(H40A,H40B), C39(H39A,H39B), C80(H80A,
 H80B), C79(H79A,H79B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C31(H31), C6(H6), C23(H23), C4(H4), C7(H7), C25(H25), C30(H30),
 C3(H3), C21(H21), C16(H16), C22(H22), C17(H17), C28(H28), C36(H36), C29(H29),
 C37(H37), C35(H35), C27(H27), C33(H33), C34(H34), C18(H18), C10(H10), C1(H1)
2.d Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C75(H75A,H75B,H75C), C56(H56A,H56B,H56C), C97(H97A,H97B,
 H97C), C57(H57A,H57B,H57C), C76(H76A,H76B,H76C), C55(H55A,H55B,H55C), C96(H96A,
 H96B,H96C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              86678
_shelx_hkl_checksum              25570
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.683