Terbium-fluorido cluster: an energy cage for photoluminescence.
Ling, Bo-Kai; Li, Junhao; Zhai, Yuan-Qi; Hsu, Hung-Kai; Chan, Yi-Tsu; Chen, Wei-Peng; Han, Tian; Zheng, Yan-Zhen; Chemical communications (Cambridge, England) 56 (2020) 9130–9133; doi:10.1039/d0cc02898c

data_7126867
_publ_section_title
;
 Terbium-fluorido cluster: an energy cage for photoluminescence.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9130
_journal_page_last               9133
_journal_paper_doi               10.1039/d0cc02898c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C73 H133 F8 N O29 Tb6'
_chemical_formula_sum            'C73 H133 F8 N O29 Tb6'
_chemical_formula_weight         2594.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.191(9)
_cell_length_b                   23.761(6)
_cell_length_c                   15.011(4)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.25
_cell_volume                     12908(6)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      150
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            81304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.7457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             5088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL pnma_a.res in Pnma
CELL   36.1910   23.7610   15.0110     90.00     90.00     90.00
SPGR Pnma
Q101 0.939 0.744 0.438 !       9.66 eA-3
Q102 0.414 0.754 0.438 !       8.93 eA-3
Q103 0.279 0.246 0.656 !       8.14 eA-3
Q104 0.870 0.823 0.268 !       7.87 eA-3
C105 0.486 0.748 0.406 !       6.87 eA-3
C106 0.511 0.247 0.125 !       6.49 eA-3
C107 0.970 0.768 0.437 !       6.47 eA-3
Q108 0.158 0.253 0.625 !       5.81 eA-3
C109 0.548 0.751 0.078 !       5.75 eA-3
C110 0.378 0.256 0.891 !       5.73 eA-3
Q111 0.975 0.835 0.282 !       5.21 eA-3
C112 0.096 0.750 0.328 !       5.10 eA-3
Q113 0.754 0.232 0.546 !       5.03 eA-3
C114 0.561 0.750 0.156 !       4.92 eA-3
Q115 0.976 0.673 0.220 !       4.40 eA-3
Q116 0.908 0.840 0.205 !       4.22 eA-3
C117 0.810 0.250 0.297 !       4.09 eA-3
C118 0.109 0.748 0.234 !       4.08 eA-3
Q119 0.302 0.839 0.326 !       4.05 eA-3
C120 0.335 0.250 0.484 !       3.90 eA-3
Q121 0.127 0.252 0.000 !       3.83 eA-3
C122 0.252 0.250 0.156 !       3.69 eA-3
Q123 0.646 0.751 0.094 !       3.54 eA-3
C124 0.350 0.252 0.531 !       3.40 eA-3
Q125 0.288 0.821 0.250 !       3.31 eA-3
C126 0.610 0.647 0.484 !       3.30 eA-3
Q127 0.871 0.921 0.046 !       3.26 eA-3
Q128 0.242 0.752 0.062 !       3.22 eA-3
Q129 0.233 0.250 0.625 !       3.16 eA-3
Q130 0.679 0.250 0.547 !       3.11 eA-3
C131 0.075 0.750 0.031 !       3.09 eA-3
Q132 0.345 0.665 0.297 !       3.02 eA-3
Q133 0.956 0.765 0.376 !       3.02 eA-3
Q134 0.847 0.580 0.406 !       2.97 eA-3
C135 0.910 0.250 0.594 !       2.95 eA-3
C136 0.934 0.250 0.250 !       2.91 eA-3
Q137 0.501 0.730 0.382 !       2.90 eA-3
C138 0.807 0.210 0.282 !       2.88 eA-3
Q139 0.438 0.536 0.496 !       2.87 eA-3
Q140 0.774 0.749 0.062 !       2.86 eA-3
C141 0.769 0.248 0.281 !       2.85 eA-3
C142 0.934 0.344 0.348 !       2.80 eA-3
Q143 0.631 0.250 0.828 !       2.80 eA-3
C144 0.448 0.284 0.468 !       2.79 eA-3
C145 0.093 0.674-0.002 !       2.75 eA-3
Q146 0.165 0.257 0.501 !       2.73 eA-3
C147 0.960 0.749 0.484 !       2.73 eA-3
C148 0.938 0.248 0.172 !       2.71 eA-3
Q149 0.695 0.250 0.000 !       2.70 eA-3
Q150 0.766 0.834 0.203 !       2.65 eA-3
C151 0.383 0.244 0.234 !       2.61 eA-3
Q152 0.737 0.248 0.125 !       2.52 eA-3
C153 0.819 0.268 0.237 !       2.51 eA-3
C154 0.610 0.749 0.984 !       2.45 eA-3
Q155 0.990 0.774 0.390 !       2.45 eA-3
C156 0.901 0.227 0.252 !       2.43 eA-3
C157 0.383 0.269 0.969 !       2.41 eA-3
Q158 0.883 0.726 0.468 !       2.40 eA-3
Q159 0.080 0.317 0.671 !       2.36 eA-3
C160 0.406 0.330 0.113 !       2.35 eA-3
C161 0.822 0.186 0.230 !       2.35 eA-3
C162 0.676 0.754 0.453 !       2.35 eA-3
Q163 0.352 0.742 0.403 !       2.32 eA-3
C164 0.538 0.827 0.846 !       2.30 eA-3
C165 0.966 0.251 0.141 !       2.30 eA-3
C166 0.472 0.751 0.609 !       2.29 eA-3
C167 0.046 0.747 0.031 !       2.29 eA-3
Q168 0.237 0.250 0.266 !       2.29 eA-3
Q169 0.807 0.749 0.422 !       2.29 eA-3
C170 0.725 0.252 0.375 !       2.28 eA-3
Q171 0.046 0.186 0.719 !       2.27 eA-3
C172 0.580 0.726 0.798 !       2.27 eA-3
C173 0.642 0.697 0.467 !       2.23 eA-3
C174 0.875 0.131 0.933 !       2.23 eA-3
C175 0.859 0.210 0.015 !       2.23 eA-3
C176 0.335 0.292 0.530 !       2.22 eA-3
C177 0.744 0.290 0.346 !       2.22 eA-3
C178 0.515 0.808 0.824 !       2.21 eA-3
Q179 0.304 0.749 0.891 !       2.21 eA-3
C180 0.513 0.749 0.469 !       2.20 eA-3
C181 0.456 0.252 0.485 !       2.20 eA-3
C182 0.696 0.665 0.894 !       2.19 eA-3
Q183 0.219 0.253 0.562 !       2.19 eA-3
C184 0.637 0.752 0.031 !       2.18 eA-3
Q185 0.816 0.649 0.283 !       2.18 eA-3
C186 0.126 0.587 0.049 !       2.17 eA-3
Q187 0.078 0.337 0.844 !       2.16 eA-3
C188 0.363 0.253 0.828 !       2.15 eA-3
C189 0.616 0.618 0.455 !       2.15 eA-3
Q190 0.158 0.749 0.172 !       2.14 eA-3
C191 0.086 0.675 0.313 !       2.14 eA-3
C192 0.533 0.772 0.030 !       2.12 eA-3
Q193 0.102 0.147 0.701 !       2.10 eA-3
Q194 0.806 0.750 0.687 !       2.09 eA-3
C195 0.983 0.762 0.503 !       2.08 eA-3
Q196 0.532 0.229 0.142 !       2.08 eA-3
C197 0.143 0.663 0.718 !       2.07 eA-3
Q198 0.524 0.336 0.340 !       2.06 eA-3
Q199 0.835 0.796 0.221 !       2.06 eA-3
;
_refine_diff_density_max         6.588
_refine_diff_density_min         -2.297
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         11657
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0980
_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^)+(0.0787P)^2^+994.4491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8037
_reflns_number_total             11657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02898c7.cif
_cod_data_source_block           pnma_sq
_cod_depositor_comments          'Adding full bibliography for 7126867.cif.'
_cod_database_code               7126867
_shelx_shelxl_version_number     2014/7
_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. Rigid bond restraints
 C01F, N00Q, C016, C019
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00F, C00S, O00E, C00X, C01H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01T, C014, C01X, C01B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01W, C27, C013, C00V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00E, O00F, C00S, C00X, C01G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C023, C01V, C01L, C010
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C018, C01N, C01J, C012
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C010 \\sim C023 \\sim C01V \\sim C01L \\sim C00Z: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C01T \\sim C014 \\sim C01X \\sim C01B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C023 \\sim C01V \\sim C01L \\sim C010: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C17 \\sim C01E \\sim C017 \\sim C024 \\sim C35 \\sim C23: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
O00F \\sim C00S \\sim O00E \\sim C00X \\sim C01G \\sim C01H \\sim C020: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C3 \\sim O5 \\sim C021 \\sim C01C \\sim C01Z \\sim C01I: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C9 \\sim C018 \\sim C01J \\sim C01N: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
F00A \\sim Tb04 \\sim F008: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O00J \\sim C00V \\sim O00C \\sim C013 \\sim C01W \\sim C01Q \\sim C27: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C01F \\sim C016 \\sim N00Q \\sim C019: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(F008) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F006) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F005) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H01D(0.5) H01E(0.5) H01F(0.5) H01J(0.5) H01K(0.5) H01L(0.5)
 O13(0.5) O12(0.5) C23(0.5) C35(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C016(H016)
5.b Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C019(H01D,H01E,H01F), C01B(H01G,H01H,H01I), C01F(H01J,
 H01K,H01L), C01G(H01M,H01N,H01O), C01H(H01P,H01Q,H01R), C01I(H01S,H01T,H01U),
 C01J(H01V,H01W,H01X), C01L(H01Y,H,HA), C01N(H01Z,HB,HC), C01Q(H01,HD,HE),
 C01T(H0AA,HF,HG), C01V(H1AA,HH,HI), C01W(H2AA,HJ,HK), C01X(H3AA,HL,HM),
 C01Z(H4AA,HN,HO), C020(H02A,H02B,H02C), C021(H02D,H02E,H02F), C023(H02G,H02H,
 H02I), C024(H02J,H02K,H02L), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C9(H9A,
 H9B,H9C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'