High circularly polarized luminescence brightness from analogues of Shibasaki's lanthanide complexes.
Deng, Min; Schley, Nathan D.; Ung, Gaël; Chemical communications (Cambridge, England) 56 (2020) 14813–14816; doi:10.1039/d0cc06568d

data_7127475
_publ_section_title
;
 High circularly polarized luminescence brightness from analogues of
 Shibasaki's lanthanide complexes.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14813
_journal_page_last               14816
_journal_paper_doi               10.1039/d0cc06568d
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C84 H108 La Na3 O12, 1.05(C4 H8 O)'
_chemical_formula_sum            'C88.19 H116.39 La Na3 O13.05'
_chemical_formula_weight         1593.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-07 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.4265(7)
_cell_length_b                   27.2114(9)
_cell_length_c                   10.4341(3)
_cell_measurement_reflns_used    18279
_cell_measurement_temperature    109(13)
_cell_measurement_theta_max      26.8200
_cell_measurement_theta_min      2.9080
_cell_volume                     8071.0(4)
_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 (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      109(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.913
_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    -42.00  11.00   0.50   20.00    --  -16.04 -77.00 -90.00  106
  2  \w    -42.00  11.00   0.50   20.00    --  -16.04 -77.00 150.00  106
  3  \w    -42.00  11.00   0.50   20.00    --  -16.04 -77.00 -30.00  106
  4  \w    -43.00  21.00   0.50   20.00    --  -16.04  77.00  60.00  128
  5  \w     -3.00  85.00   0.50   20.00    --   16.11  38.00 -90.00  176
  6  \w      3.00  32.00   0.50   20.00    --   16.11  57.00   0.00   58
  7  \w     46.00  72.00   0.50   20.00    --   16.11   0.00 120.00   52
  8  \w    -49.00   4.00   0.50   20.00    --   16.11   0.00 120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0133307000
_diffrn_orient_matrix_UB_12      -0.0031120000
_diffrn_orient_matrix_UB_13      -0.0568761000
_diffrn_orient_matrix_UB_21      0.0052807000
_diffrn_orient_matrix_UB_22      0.0245073000
_diffrn_orient_matrix_UB_23      -0.0183091000
_diffrn_orient_matrix_UB_31      0.0204131000
_diffrn_orient_matrix_UB_32      -0.0083681000
_diffrn_orient_matrix_UB_33      -0.0323637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            75037
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.431
_diffrn_reflns_theta_min         2.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.227
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 5295 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         19396
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+10.8832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                16081
_reflns_number_total             19396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06568d2.cif
_cod_data_source_block           nd-603
_cod_database_code               7127475
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C84H101LaNa3O12
_reflns_odcompleteness_completeness 99.49
_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, All C(H,H,H,H) groups
2. Restrained distances
 C53-C54 \\sim C53-C54A
 with sigma of 0.02
 C56-C55 \\sim C56-C55A
 with sigma of 0.02
 C55-C54 \\sim C55A-C54A
 with sigma of 0.02
 C53-C55 \\sim C53-C55A
 with sigma of 0.04
 C56-C54 \\sim C56-C54A
 with sigma of 0.04
 C77-C78 \\sim C77-C78A
 with sigma of 0.02
 C78-C79 \\sim C78A-C79
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C54 \\sim C54A \\sim C55 \\sim C55A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C78 \\sim C78A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
O13 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O14 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55C)=
 Sof(H55D)=Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(H56A)=Sof(H56B)=FVAR(1)
 Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=Sof(H79C)=Sof(H79D)=1-FVAR(2)
 Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H79A)=Sof(H79B)=FVAR(2)
 Sof(O13)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=FVAR(3)
 Sof(O14)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=
 Sof(H1GA)=Sof(H1GB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=FVAR(4)
5.a Free rotating group:
 O13(C1A,C1B,C1C,C1D), O14(C1E,C1F,C1G,C1H)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C53(H53A,H53B), C53(H53C,H53D), C54(H54A,H54B), C54A(H54C,H54D),
 C55(H55A,H55B), C55A(H55C,H55D), C56(H56A,H56B), C56(H56C,H56D), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C77(H77C,H77D), C78(H78A,H78B),
 C78A(H78C,H78D), C79(H79A,H79B), C79(H79C,H79D), C80(H80A,H80B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C1A(H1AA,H1AB),
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1F(H1FA,H1FB),
  C1G(H1GA,H1GB), C1H(H1HA,H1HB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C13(H13), C14(H14), C22(H22), C23(H23), C38(H38), C39(H39),
 C42(H42), C43(H43), C58(H58), C59(H59)
;
_shelx_res_checksum              15293
_olex2_date_sample_data_collection 2020-08-29
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide 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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.773