Electronic strain effect on Eu(iii) complexes for enhanced circularly polarized luminescence.
Tsurui, Makoto; Kitagawa, Yuichi; Fushimi, Koji; Gon, Masayuki; Tanaka, Kazuo; Hasegawa, Yasuchika; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5352–5361; doi:10.1039/d0dt00699h

data_7703850
_publ_section_title
;
 Electronic strain effect on Eu(iii) complexes for enhanced circularly
 polarized luminescence.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5352
_journal_page_last               5361
_journal_paper_doi               10.1039/d0dt00699h
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'0.5(C33 H31 Eu F18 N2 O8 P2), 0.5(C32.37 H31 Eu F18 N2 O8 P2)'
_chemical_formula_sum            'C33 H31 Eu F18 N2 O8 P2'
_chemical_formula_weight         1139.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.568(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6679(3)
_cell_length_b                   19.2967(4)
_cell_length_c                   20.2075(4)
_cell_measurement_reflns_used    44508
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      29.5570
_cell_measurement_theta_min      2.3400
_cell_volume                     4540.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_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_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_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    -71.00  31.00   0.50    7.97    --    0.00  29.00 -30.00  204
  2  \w     47.00  74.00   0.50    7.97    --    0.00  29.00 -30.00   54
  3  \w    -44.00  89.00   0.50    7.97    --    0.00  14.00-180.00  266
  4  \w    -54.00 -28.00   0.50    7.97    --    0.00  43.00  90.00   52
  5  \w     35.00  73.00   0.50    7.97    --    0.00  43.00  90.00   76
  6  \w     -2.00  23.00   0.50    7.97    --    0.00  57.00-120.00   50
  7  \w     64.00  89.00   0.50    7.97    --    0.00  57.00-120.00   50
  8  \w    -65.00 -37.00   0.50    7.97    --    0.00  43.00 -30.00   56
  9  \w     28.00  54.00   0.50    7.97    --    0.00  43.00 -30.00   52
 10  \w      8.00  34.00   0.50    7.97    --    0.00  57.00  60.00   52
 11  \w    -23.00  16.00   0.50    7.97    --    0.00  57.00 120.00   78
 12  \w    -71.00 -45.00   0.50    7.97    --    0.00  57.00 150.00   52
 13  \w    -54.00 -29.00   0.50    7.97    --    0.00  43.00-180.00   50
 14  \w    -56.00   1.00   0.50    7.97    --    0.00  60.00-162.36  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0583125000
_diffrn_orient_matrix_UB_12      0.0105204000
_diffrn_orient_matrix_UB_13      -0.0034154000
_diffrn_orient_matrix_UB_21      0.0160970000
_diffrn_orient_matrix_UB_22      0.0338647000
_diffrn_orient_matrix_UB_23      0.0106531000
_diffrn_orient_matrix_UB_31      0.0071045000
_diffrn_orient_matrix_UB_32      0.0097180000
_diffrn_orient_matrix_UB_33      -0.0333318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            108043
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.445
_diffrn_reflns_theta_min         2.020
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_refine_diff_density_max         1.833
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 8771 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1552
_refine_ls_number_reflns         22733
_refine_ls_number_restraints     1176
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0661P)^2^+4.2163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                20369
_reflns_number_total             22733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00699h2.cif
_cod_data_source_block           EuhfaSS-B2QPO
_cod_depositor_comments
'Adding full bibliography for 7703848--7703853.cif.'
_cod_database_code               7703850
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P O F Eu'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C03J-C03I = C5-C03I
 1.56 with sigma of 0.02
 F3-C1 = F2-C1 = F6-C1
 1.32 with sigma of 0.01
 F16-C6 = F15-C6 = F14-C6
 1.32 with sigma of 0.01
 C3-C69
 1.56 with sigma of 0.02
 F10-C3 = F8-C3 = F9-C3
 1.32 with sigma of 0.02
 F9-F8 = F9-F10
 2.1 with sigma of 0.02
 F8-F10
 2.1 with sigma of 0.02
 C1-C30
 1.56 with sigma of 0.02
 Eu02-O00R = Eu02-O00D = Eu02-O007 = Eu02-O00C = Eu02-O012 = Eu02-O00A = Eu02-
 O009
 2.38 with sigma of 0.01
 O007-C41
 1.24 with sigma of 0.02
 C5AA-C3AA
 1.56 with sigma of 0.02
 C3AA-C03K = C5A-C3AA
 1.56 with sigma of 0.02
 F02R-C01Y = F02F-C01Y = F030-C01Y = F3AA-C036 = F1-C036 = F2AA-C036 = F037-
 C02A = F038-C02A = F03A-C02A
 1.32 with sigma of 0.01
 C03I-C03G
 2.96 with sigma of 0.02
 P006-C03G
 1.8 with sigma of 0.02
 C03C-C03I
 1.56 with sigma of 0.02
 C03I-C03J \\sim C3AA-C03K
 with sigma of 0.02
 C03I-C5 \\sim C3AA-C5A
 with sigma of 0.02
 C03J-C5 \\sim C03K-C5A
 with sigma of 0.04
 C02U-C035 \\sim C02V-C0
 with sigma of 0.02
 C02U-C9 \\sim C02V-C9A
 with sigma of 0.02
 C035-C9 \\sim C0-C9A
 with sigma of 0.04
 P006-C03I \\sim P006-C3AA
 with sigma of 0.02
 P006-C03J \\sim P006-C03K
 with sigma of 0.04
 P006-C5 \\sim P006-C5A
 with sigma of 0.04
 P005-C02U \\sim P005-C02V
 with sigma of 0.02
 P005-C035 \\sim P005-C0
 with sigma of 0.04
 P005-C9 \\sim P005-C9A
 with sigma of 0.04
 C02B-C02U \\sim C02C-C02V
 with sigma of 0.02
 C02B-C035 \\sim C02C-C0
 with sigma of 0.04
 C02B-C9 \\sim C02C-C9A
 with sigma of 0.04
 P005-C02B \\sim P005-C02C
 with sigma of 0.04
 C03C-C03I \\sim C5AA-C3AA
 with sigma of 0.02
 C03C-C03J \\sim C5AA-C03K
 with sigma of 0.04
 C03C-C5 \\sim C5AA-C5A
 with sigma of 0.04
 P006-C03C \\sim P006-C5AA
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O009 \\sim O00C \\sim C01G \\sim C025 \\sim C02M \\sim C02Y \\sim F02L \\sim
F02X \\sim F65 \\sim F037 \\sim C02A \\sim F038 \\sim F03A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
O012 \\sim C30 \\sim F3 \\sim C1 \\sim F2 \\sim F6 \\sim C52 \\sim C69 \\sim
O009 \\sim C3 \\sim F10 \\sim F8 \\sim F9: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
F14 \\sim C6 \\sim F16 \\sim F15 \\sim C41 \\sim O007 \\sim C36 \\sim C0AA
\\sim O0 \\sim C4 \\sim F13 \\sim F11 \\sim F12: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
F1E \\sim C10 \\sim F1F \\sim F4 \\sim C02D \\sim C01C \\sim C020 \\sim F02F
\\sim C01Y \\sim F02R \\sim F030 \\sim O012: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C02B \\sim C02U \\sim C9 \\sim C035 \\sim P005: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
P006 \\sim C3AA \\sim C5AA \\sim C5A \\sim C03K: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
C9A \\sim C02V \\sim C02C \\sim C0 \\sim P005: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
O00C \\sim C14 \\sim C1AA \\sim C8 \\sim F1AA \\sim F1C \\sim F1A \\sim C17
\\sim O00A \\sim F19 \\sim F4AA \\sim F17 \\sim C7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
O00A \\sim C02O \\sim F7 \\sim F5 \\sim F0AA \\sim C02J \\sim C02K \\sim O007
\\sim C036 \\sim F2AA \\sim F3AA \\sim F1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C03G \\sim P006 \\sim C03I \\sim C03J \\sim C5: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
C03C \\sim C03I \\sim C03J \\sim C5 \\sim P006 \\sim C03G: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O009, O00C, C01G, C025, C02M, C02Y, F02L, F02X, F65, F037, C02A, F038, F03A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O012, C30, F3, C1, F2, F6, C52, C69, O009, C3, F10, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0, C0AA, C4, F13, F11, F12, C36, C41, O007, C6, F15, F14, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C02B, C02U, C9, C035, P005
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P006, C3AA, C5AA, C5A, C03K
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9A, C02C, C02V, C0, P005, C4AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4AA, F17, C7, F19, C17, O00A, C1AA, C14, C8, F1A, F1C, F1AA, O00C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1, F2AA, C036, F3AA, C02K, O007, C02J, C02O, F7, C7, F5, F0AA, O00A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C03G, P006, C03I, C03J, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C03G, P006, C03J, C03I, C5, C03C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C0AA)=Sof(C30)=Sof(C36)=Sof(H36)=Sof(C41)=Sof(C52)=Sof(H52)=Sof(C69)=
 Sof(C1)=Sof(F3)=Sof(F2)=Sof(F6)=Sof(C3)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(C4)=
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(C6)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(C14)=
 Sof(C17)=Sof(F1AA)=Sof(C7)=Sof(F17)=Sof(F19)=Sof(C8)=Sof(F1A)=Sof(F1C)=
 Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(F4AA)=Sof(C1AA)=Sof(H1AA)=1-FVAR(1)
 Sof(C01C)=Sof(H01G)=Sof(C01G)=Sof(C01Y)=Sof(C020)=Sof(C025)=Sof(H025)=
 Sof(C02A)=Sof(C02D)=Sof(F02F)=Sof(C02J)=Sof(H02V)=Sof(C02K)=Sof(F02L)=
 Sof(C02M)=Sof(C02O)=Sof(F02R)=Sof(F02X)=Sof(C02Y)=Sof(F030)=Sof(C032)=
 Sof(H03A)=Sof(H03B)=Sof(H03C)=Sof(C036)=Sof(F037)=Sof(F038)=Sof(F03A)=
 Sof(C03G)=Sof(H03M)=Sof(H03N)=Sof(H03O)=Sof(F1)=Sof(F2AA)=Sof(F3AA)=Sof(C10)=
 Sof(F4)=Sof(F1E)=Sof(F1F)=Sof(F65)=Sof(F0AA)=Sof(F5)=Sof(F7)=FVAR(1)
 Sof(C3AA)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C5A)=Sof(H5AD)=
 Sof(H5AE)=Sof(H5AF)=Sof(C03K)=Sof(H03R)=Sof(H03S)=Sof(H03T)=1-FVAR(2)
 Sof(C03C)=Sof(H03G)=Sof(H03I)=Sof(H03J)=Sof(C03I)=Sof(C03J)=Sof(H03P)=
 Sof(H03Q)=Sof(H03U)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
 Sof(C02V)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C02C)=Sof(H02D)=
 Sof(H02E)=Sof(H02F)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=1-FVAR(3)
 Sof(C02B)=Sof(H02S)=Sof(H02T)=Sof(H02U)=Sof(C02U)=Sof(C035)=Sof(H03D)=
 Sof(H03E)=Sof(H03F)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(3)
6.a Free rotating group:
 C10(F4,F1E,F1F)
6.b Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C010(H010), C013(H013), C01C(H01G), C01M(H01M), C01P(H01P),
 C024(H024), C025(H025), C029(H029), C02J(H02V), C02Z(H02Z), C03D(H03K),
 C03F(H03L), C03H(H03H), C36(H36), C52(H52), C1AA(H1AA)
6.c Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C01Q(H01A,H01B,H01C), C01V(H01D,H01E,H01F), C021(H02A,
 H02B,H02C), C022(H02G,H02H,H02I), C026(H02J,H02K,H02L), C02B(H02S,H02T,H02U),
 C02I(H02M,H02N,H02O), C02S(H02P,H02Q,H02R), C032(H03A,H03B,H03C), C035(H03D,
 H03E,H03F), C03C(H03G,H03I,H03J), C03G(H03M,H03N,H03O), C03J(H03P,H03Q,H03U),
 C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C2AA(H2AA,H2AB,H2AC), C4AA(H4AA,H4AB,H4AC),
 C5AA(H5AA,H5AB,H5AC), C5A(H5AD,H5AE,H5AF), C03K(H03R,H03S,H03T), C9A(H9AA,H9AB,
 H9AC), C02C(H02D,H02E,H02F), C0(H0A,H0B,H0C)
;
_shelx_res_checksum              26536
_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 3.672
_oxdiff_exptl_absorpt_empirical_full_min 0.255