Long-lived emission beyond 1000 nm: control of excited-state dynamics in a dinuclear Tb(III)-Nd(III) complex.
Kitagawa, Yuichi; Matsuda, Kenji; da Rosa, Pedro Paulo Ferreira; Fushimi, Koji; Hasegawa, Yasuchika; Chemical communications (Cambridge, England) 57 (2021) 8047–8050; doi:10.1039/d1cc03596g

data_7128682
_publ_section_title
;
 Long-lived emission beyond 1000 nm: control of excited-state dynamics in
 a dinuclear Tb(III)-Nd(III) complex.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8047
_journal_page_last               8050
_journal_paper_doi               10.1039/d1cc03596g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C141 H204 O21 P3 Tb3'
_chemical_formula_sum            'C141 H204 O21 P3 Tb3'
_chemical_formula_weight         2804.70
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-16 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3827(3)
_cell_length_b                   22.9977(4)
_cell_length_c                   38.2920(6)
_cell_measurement_reflns_used    63392
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0110
_cell_measurement_theta_min      1.8120
_cell_volume                     15307.7(4)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.898
_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      5.00  30.00   0.50   27.45    --    5.00  21.00-105.00   50
  2  \w    -32.00  -7.00   0.50   27.45    --   -7.20  21.00-105.00   50
  3  \w     20.00  46.00   0.50   27.45    --    5.00  29.00 -60.00   52
  4  \w    -97.00 -16.00   0.50   27.45    --   -7.20  29.00 150.00  162
  5  \w     38.00  64.00   0.50   27.45    --   -7.20  29.00 150.00   52
  6  \w      9.00  82.00   0.50   27.45    --   -7.20  29.00  90.00  146
  7  \w    -94.00 -66.00   0.50   27.45    --   -7.20  29.00  90.00   56
;
_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      -0.0293401000
_diffrn_orient_matrix_UB_12      -0.0107145000
_diffrn_orient_matrix_UB_13      -0.0111719000
_diffrn_orient_matrix_UB_21      0.0249787000
_diffrn_orient_matrix_UB_22      0.0029335000
_diffrn_orient_matrix_UB_23      -0.0145473000
_diffrn_orient_matrix_UB_31      0.0134136000
_diffrn_orient_matrix_UB_32      -0.0287626000
_diffrn_orient_matrix_UB_33      0.0026543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            124097
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.027
_diffrn_reflns_theta_min         1.813
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81345
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       prism
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 11734 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.498(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1570
_refine_ls_number_reflns         35085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+9.9294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.816
_reflns_number_gt                29895
_reflns_number_total             35085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03596g2.cif
_cod_data_source_block           tbtmhdpppo
_cod_depositor_comments
'Adding full bibliography for 7128682--7128683.cif.'
_cod_database_code               7128682
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O P Tb'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.593
_reflns_odcompleteness_completeness 99.84
_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.a Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C012(H012), C014(H014), C017(H017), C019(H019), C01A(H01A),
 C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H01H),
 C01I(H01I), C01J(H01J), C01N(H01N), C01P(H01P), C01R(H01R), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C024(H024), C02A(H02D),
 C02B(H02E), C02D(H02F), C02G(H02G), C02I(H02I), C02J(H02J), C02P(H02P),
 C02Q(H02Q), C02V(H02V), C02W(H02W), C02X(H02X), C031(H031), C03F(H0AA),
 C03Q(H0BA), C03T(H3BA), C041(H041), C044(H044), C04F(H9BA)
2.b Idealised Me refined as rotating group:
 C027(H02A,H02B,H02C), C02K(H02H,H02K,H02L), C02L(H02M,H02N,H02O), C02U(H02R,
 H02S,H02T), C02Y(H02U,H02Y,H), C030(H03A,H03B,H03C), C032(H03D,H03E,H03F),
 C033(H03G,H03H,H03I), C035(H03J,H03K,H03L), C037(H03M,H03N,H03O), C038(H03P,
 H03Q,H03R), C039(H03S,H03T,H03U), C03A(H03V,H03W,H03X), C03B(H03Y,HA,HB),
 C03C(H03Z,HC,HD), C03E(H03,HE,HF), C03G(H1AA,HG,HH), C03H(H2AA,HI,HJ),
 C03I(H3AA,HK,HL), C03K(H4AA,HM,HN), C03L(H5AA,HO,HP), C03M(H6AA,HQ,HR),
 C03N(H7AA,HS,HT), C03O(H8AA,HU,HV), C03P(H9AA,HW,HX), C03R(H1BA,HY,HZ),
 C03S(H2BA,H7CA,H8CA), C03U(H4BA,H9CA,H0DA), C03V(H5BA,H1DA,H2DA), C03W(H6BA,
 H3DA,H4DA), C03X(H7BA,H5DA,H6DA), C03Z(H8BA,H7DA,H8DA), C040(H04A,H04B,H04C),
 C042(H04D,H04E,H04F), C043(H04G,H04H,H04I), C045(H04J,H04K,H04L), C046(H04M,
 H04N,H04O), C047(H04P,H04Q,H04R), C049(H04S,H04T,H04U), C04A(H04V,H04W,H04X),
 C04C(H04Y,H9DA,H0EA), C04D(H04Z,H1EA,H2EA), C04E(H04,H3EA,H4EA), C04G(H0CA,
 H5EA,H6EA), C04H(H1CA,H7EA,H8EA), C04I(H2CA,H9EA,H0FA), C04K(H3CA,H1FA,H2FA),
 C04M(H4CA,H3FA,H4FA), C04O(H5CA,H5FA,H6FA), C04P(H6CA,H7FA,H8FA), C11(H11A,
 H11B,H11C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              95191
_shelx_hkl_checksum              75242
_shelx_fab_checksum              47415
_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 3.798
_oxdiff_exptl_absorpt_empirical_full_min 0.353